CN110142024A - A kind of method and its application preparing N doping multiporous biological charcoal using abandoned biomass - Google Patents
A kind of method and its application preparing N doping multiporous biological charcoal using abandoned biomass Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000002028 Biomass Substances 0.000 title claims abstract description 31
- 239000003610 charcoal Substances 0.000 title abstract description 5
- 239000000243 solution Substances 0.000 claims abstract description 57
- 239000000463 material Substances 0.000 claims abstract description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 41
- 239000000843 powder Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 31
- 238000001179 sorption measurement Methods 0.000 claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 20
- 238000010521 absorption reaction Methods 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 10
- 238000002604 ultrasonography Methods 0.000 claims abstract description 10
- 238000010792 warming Methods 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 244000241235 Citrullus lanatus Species 0.000 claims abstract description 4
- 235000012828 Citrullus lanatus var citroides Nutrition 0.000 claims abstract description 4
- 235000005979 Citrus limon Nutrition 0.000 claims abstract description 4
- 244000131522 Citrus pyriformis Species 0.000 claims abstract description 4
- 240000006053 Garcinia mangostana Species 0.000 claims abstract description 4
- 235000017048 Garcinia mangostana Nutrition 0.000 claims abstract description 4
- 240000008790 Musa x paradisiaca Species 0.000 claims abstract description 3
- 235000018290 Musa x paradisiaca Nutrition 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 238000002474 experimental method Methods 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 241000609240 Ambelania acida Species 0.000 claims description 3
- 240000000716 Durio zibethinus Species 0.000 claims description 3
- 235000006025 Durio zibethinus Nutrition 0.000 claims description 3
- 239000010905 bagasse Substances 0.000 claims description 3
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 244000183278 Nephelium litchi Species 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 210000000582 semen Anatomy 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims 1
- 239000004698 Polyethylene Substances 0.000 claims 1
- 239000004743 Polypropylene Substances 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 229960003431 cetrimonium Drugs 0.000 claims 1
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 claims 1
- -1 polyethylene Polymers 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 229920001155 polypropylene Polymers 0.000 claims 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 229920000428 triblock copolymer Polymers 0.000 claims 1
- 239000011651 chromium Substances 0.000 abstract description 13
- 239000010949 copper Substances 0.000 abstract description 12
- 238000002360 preparation method Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052793 cadmium Inorganic materials 0.000 abstract description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 230000009102 absorption Effects 0.000 description 17
- 239000002351 wastewater Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000010828 animal waste Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010814 metallic waste Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (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 invention discloses a kind of method and its application that N doping multiporous biological charcoal is prepared using abandoned biomass.Using biomass such as the extensive mangosteen skin in source, lemon peel, watermelon peel, banana skins as raw material, heavy metal in the material energy efficient removal water prepared by template and hydro-thermal method.The following steps are included: 1) pericarp is cleaned dries pulverizing, the aqueous solution dissolved with nitrogen source and the ethanol solution dissolved with template are sequentially added, is stirred after ultrasound；2) solution is transferred in hydrothermal reaction kettle and is heated to 140 DEG C of 6 h of holding, cooled down and be dried in vacuo after taking-up；3) by solid abrasive at powder, then 400 ~ 700 DEG C of 2 h of holding are warming up to the heating rate of 2 ~ 10 DEG C/min under nitrogen atmosphere, are then cooled to room temperature；4) sample with ethanol and water are respectively washed 3 times, are dried in vacuo, obtain the N doping biological carbon materials of high absorption property.The material short preparation period, process is easy, for adsorbing the heavy metals such as the lead in water (Pb [II]), copper (Cu [II]), chromium (Cr [VI]), cadmium (Cd [II]), adsorption efficiency is high, reusable.
Description
Technical field
The invention belongs to environmentally conscious materials technical fields and biomass as resources field, and in particular to a kind of to utilize waste biomass
The method and its application in terms of adsorbing heavy metal that matter prepares N doping multiporous biological charcoal.
Background technique
As industrial power, the annual discharged volume of industrial waste water in China reaches 20,000,000,000 tons or more, wherein the waste water of large number of rows
In all contain in heavy metal ion, such as electroplating wastewater containing a large amount of Cd (II), Pb (II) heavy metal；In leather industry, tan
Contain a large amount of Cr (VI) in the waste water in stage processed；Contain more heavy metal Cu (II) in acidic mine waste water.These huge sum of moneys
If category waste water is untreated, ecology in water can be endangered, and enter soil, atmosphere by the ecological circulation of the earth, finally endanger people
The health of class.Heavy metal is done great harm to human body, its almost non-degradable can be enriched with, the heavy metal of denier is just in vivo
The injury that can not be reversed can be caused to animals and plants and human body.Current process for treating heavy-metal waste water both domestic and external mainly includes chemistry
The precipitation method, chelating precipitation (flocculation) method, ion-exchange and electrochemical process etc., every kind of method all has some disadvantages.Chemistry
The precipitation method and chelate precipitation need to add excessive medicament, though eliminating heavy metal, can bring new pollution problem；Ion
Exchange process needs expensive ion exchange column, and the operating cost that electrochemical process needs is higher.Therefore, the huge sum of money in waste water is studied
Belong to processing method to be of great significance.
Biomass resource is very huge, and common includes the agriculture and forestry organic waste materials such as stalk, pericarp, also there is animal wastes, deposition
Object and sludge etc..This kind of resource yield is big, but for a long time, the mankind do not give enough attention.In fact, big at this stage
Most biomass resources are not all used effectively, or take and directly burn this more inefficient utilization means.China's agriculture
The yield of the plant waste of woods production is up to 2,000,000,000 t, but utilization efficiency is less than 30%.Most of agricultural abandoned biomass moneys
A large amount of cellulose, hemicellulose and lignin are contained in source, and cellular structure can be generated under conditions of high temperature pyrolysis, there is absorption water
The potentiality of weight metal.Study carefully its crucial technology of preparing, there is pyrolysis pore-creating excessive velocities and non-uniform disadvantage, direct high temperature
Be pyrolyzed obtained material cannot effectively its structure of regulation, and then affect the adsorption effect to heavy metal.So accomplishing have
Effect regulation prepares porous carbon material, and making biomass efficient recycling is still the existing challenge of a reality.
Summary of the invention
In view of the above heavy metal pollution and biomass solid waste high efficient resourcing problem, the present invention in water body lead, copper,
The heavy metals such as chromium, cadmium, it is desirable to provide a kind of utilization method of biomass solid waste high efficient resourcing, while solving heavy metal pollution and asking
Topic.
The main purpose of the present invention is to provide a kind of methods for preparing N doping multiporous biological charcoal using abandoned biomass
And its application.The present invention is guided using template as structure, forms porous microstructure by hydro-thermal pyrolysis processing, greatly
The specific surface area for improving material assigns its ability for adsorbing heavy metal ion.The nitrogenous function that material surface generates after N doping
Group generates electrostatic interaction and coordination with heavy metal ion, significantly enhances the adsorption capacity of material
The multiporous biological matter Carbon Materials for preparing N doping are combined present invention firstly provides template and hydro-thermal pyrolysismethod, and can
The efficiently contents of many kinds of heavy metal ion in removal water body.The method is low in cost, easy to operate, the material adsorption effect prepared
It is superior, there is stronger industrial applications prospect, specifically includes the following steps:
(1) first pericarp (such as mangosteen skin, lemon peel, watermelon peel, durian shell, semen litchi and bagasse) is dried, then uses crusher
With ball mill grinding at 1 g powder is weighed after powder, sequentially adding 10 mL, (urea or ethylenediamine, 0.2 ~ 0.5 g) dissolved with nitrogen source
Aqueous solution, dissolved with template, (P123 or CTAB, 0.02 ~ 0.05 ethanol solution g) stir 12 h after 1 h of ultrasound to 5 mL.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with 2 ~ 10 DEG C/min's
Heating rate is warming up to 400 ~ 700 DEG C, keeps 2 h, is then cooled to room temperature,
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high absorption property
N doping biological carbon materials.
The biological carbon materials that this technology is invented are added into the aqueous solution containing heavy metal ion, in churned mechanically work
With lower its adsorption process of promotion, pH, temperature are adjusted, specifically includes the following steps:
(5) 25 mL are accurately prepared with deionized water contains 50 mg/L heavy metal ion (Pb [II], Cu [II], Cr [VI] or Cd
[II]) solution, adjust its pH(2.0 ~ 8.0) after be transferred in 50 mL conical flasks.
(6) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into constant-temperature table
(15,25 or 35 DEG C of temperature) shakes the filtering of 30 min caudacorias, separation material and solution under 200 rpm revolving speeds.
Material after separation utilizes again, circulation absorption comprising following steps:
(7) material that will filter out is added in the HNO3 solution of 1 mol/L, 12 h of mechanical stirring, then is rinsed with deionized water
To neutrality, desorption is completed in vacuum drying.
(8) 25 mL are accurately prepared with deionized water contains 50 mg/L heavy metal ion (Pb [II], Cu [II], Cr [VI]
Or Cd [II]) solution, it is consistent with the pH value of solution of first adsorption experiment to adjust its pH() after be transferred in 50 mL conical flasks.
(9) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into constant-temperature table,
The filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) the N doping multiporous biological matter Carbon Materials prepared have fast and efficiently absorption property.
(2) raw material of the invention is discarded agricultural solid biomass, and from a wealth of sources low in cost, preparation method is simple, tool
There is good prospects for commercial application.
(3) the N doping multiporous biological matter Carbon Materials prepared by can be recycled for multiple times after desorption is handled.
(4) the N doping multiporous biological matter Carbon Materials prepared are degradable, facilitate processing, are not likely to produce secondary pollution.
(5) present invention solves the problems, such as that Heavy Metals in Waters removing and biomass resource efficiently utilize two overall situation simultaneously.
Detailed description of the invention
Fig. 1 is of the invention to prepare N doping multiporous biological Carbon Materials flow diagram
Wherein, 1, the pericarp taken, 2, preprocessing process (cleaning, dry, broken), 3, plant powder, 4, containing template
Ethanol solution, 5, the aqueous solution containing nitrogen source, 6, mixing, 7, hydro-thermal pyrolysis, 8, high temperature pyrolysis, 9, biomass carbon material.
Fig. 2, Fig. 3 and Fig. 4 are respectively the scanning electron microscope (SEM) photograph for the biomass carbon material being prepared in embodiment 1,2 and 3.
Fig. 5 is the transmission electron microscope picture for the biomass carbon material being prepared in embodiment 3.
Fig. 6 is that adsorption capacity changes with time when MPC-0.2U-0.02P-2400 material adsorbs Pb (II) in embodiment 7
Point and line chart.
Fig. 7 is to have adsorbed its absorption Pb (II) appearance of the MPC-0.2U-0.02P-2400 material of Pb (II) in embodiment 8 for the first time
Amount is with the variation histogram for recycling son's wife's number.
Specific embodiment
The present invention is furtherd elucidate below by drawings and examples.Following embodiment is only used for clearly saying
Bright technical solution of the present invention, therefore it is intended only as example, and cannot be limited the scope of the invention with this.
The experimental material used in following embodiments can obtain unless otherwise specified from commercial channel.
Embodiment 1: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
(1) first mangosteen skin is dried, then sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
Dissolved with the aqueous solution of 0.2 g urea, 5 mL stir 12 h after 1 h of ultrasound dissolved with the ethanol solution of 0.02 g P123.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 2 DEG C/min
Rate is warming up to 400 DEG C, keeps 2 h, is then cooled to room temperature,
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high absorption property
N doping biological carbon materials MPC-0.2U-0.02P-2400.
Embodiment 2: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) first lemon peel is dried, then sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
Dissolved with the aqueous solution of 0.5 g urea, the ethanol solution of 5 mL0.05 g P123 stirs 12 h after 1 h of ultrasound.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 5 DEG C/min
Rate is warming up to 400 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials LPC-0.5U-0.05P-5400 of energy.
Embodiment 3: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) first watermelon peel is dried, then sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
Dissolved with the aqueous solution of 0.5 g ethylenediamine, 5 mL stir 12 h after 1 h of ultrasound dissolved with the ethanol solution of 0.02 CTAB.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the liter of 10 DEG C/min
Warm rate is warming up to 700 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials WPC-0.5E-0.02C-10700 of energy.
Embodiment 4: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) first durian shell is dried, then sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
Dissolved with the aqueous solution of 0.2 g ethylenediamine, the ethanol solution of 5 mL0.05 g P123 stirs 12 h after 1 h of ultrasound.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 8 DEG C/min
Rate is warming up to 500 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials DPC-0.2E-0.05P-8500 of energy.
Embodiment 5: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) banana skin is dried, then it is molten sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
There is an aqueous solution of 0.3 g urea, 5 mL stir 12 h after 1 h of ultrasound dissolved with the ethanol solution of 0.05 CTAB.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 2 DEG C/min
Rate is warming up to 500 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials BPC-0.3U-0.05C-2500 of energy.
Embodiment 6: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) bagasse is dried, then it is molten sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
There is an aqueous solution of 0.3 g urea, 5 mL stir 12 h after 1 h of ultrasound dissolved with the ethanol solution of 0.03 CTAB.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 2 DEG C/min
Rate is warming up to 700 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials SPC-0.3U-0.03C-2700 of energy
Embodiment 7: this example provides a kind of preparation method of N doping multiporous biological matter Carbon Materials for adsorbing heavy metal
Itself the following steps are included:
(1) peanut shell is dried, then it is molten sequentially adds 10 mL at 1 g powder is weighed after powder with crusher and ball mill grinding
There is an aqueous solution of 0.5 g urea, 5 mL stir 12 h after 1 h of ultrasound dissolved with the ethanol solution of 0.03 CTAB.
(2) solution of step (1) is transferred in hydrothermal reaction kettle and carries out 140 DEG C of hydro-thermal process and keeps 6 h.After taking-up
It is cooled to room temperature and mixture is dry in vacuum oven.
(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere with the heating of 5 DEG C/min
Rate is warming up to 500 DEG C, keeps 2 h, is then cooled to room temperature.
(4) it by sample grind into powder, then is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo, obtains high adsorption
The N doping biological carbon materials PPC-0.5U-0.03C-5500 of energy
Embodiment 8: this example, which is provided, carries out Pb in water (II) using the MPC-0.2U-0.02P-2400 material in embodiment 1
The method adsorbed for the first time
Itself the following steps are included:
(1) Pb (II) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is transferred to 50 after adjusting its pH=2.0
In mL conical flask.
(2) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 15 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.Experiment only needs 20 min just to reach balance, counts
Obtained equilibrium adsorption capacity is 112 mg/g, adsorption rate 89.6%.
Embodiment 9: this example is provided using the MPC-0.2U-0.02P-2400 for having adsorbed Pb (II) in embodiment 8 for the first time
Method of the material to Pb in water (II) circulation absorption
Itself the following steps are included:
(1) the MPC-0.2U-0.02P-2400 material for having adsorbed Pb (II) in embodiment 8 for the first time is added to 1 mol/L's
In HNO3 solution, 12 h of mechanical stirring, then rinsed with deionized water to neutrality, desorption is completed in vacuum drying.
(2) Pb (II) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is shifted after adjusting its pH=2.0
Into 50 mL conical flasks.
(3) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 15 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.
And so on, complete the third of LPC-0.5U-0.05P-5400 material in embodiment 1, the 4th and the 5th absorption.
Through 5 circulation absorptions, adsorbance still reaches 97.2 mg/g.
Embodiment 10: this example is provided using the LPC-0.5U-0.05P-5400 material in embodiment 2 to Cu in water (II)
The method adsorbed for the first time
Itself the following steps are included:
(1) Cu (II) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is transferred to 50 after adjusting its pH=4.0
In mL conical flask.
(2) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 25 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.Experiment only needs 15 min just to reach balance, counts
Obtained equilibrium adsorption capacity is 119.9 mg/g, adsorption rate 95.9%.
Embodiment 11: this example is provided using the LPC-0.5U-0.05P- for having adsorbed Cu (II) in embodiment 10 for the first time
Method of 5400 materials to Cu in water (II) circulation absorption
Itself the following steps are included:
(1) the LPC-0.5U-0.05P-5400 material for having adsorbed Cu (II) in embodiment 10 for the first time is added to 1 mol/L's
In HNO3 solution, 12 h of mechanical stirring, then rinsed with deionized water to neutrality, desorption is completed in vacuum drying.
(2) Cu (II) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is shifted after adjusting its pH=4.0
Into 50 mL conical flasks.
(3) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 25 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.
And so on, complete the third of LPC-0.5U-0.05P-5400 material in embodiment 2, the 4th and the 5th absorption.
Through 5 circulation absorptions, adsorbance still reaches 108.3 mg/g.
Embodiment 12: this example is provided using the WPC-0.5E-0.02C-10700 material in embodiment 3 to Cr in water
(VI) method adsorbed for the first time
Itself the following steps are included:
(1) Cr (VI) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is transferred to 50 after adjusting its pH=2.0
In mL conical flask.
(2) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 35 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.Experiment only needs 25 min just to reach balance, counts
Obtained equilibrium adsorption capacity is 98.3 mg/g, adsorption rate 78.6%.
Embodiment 13: this example is provided using the WPC-0.5E-0.02C- for having adsorbed Cr (VI) in embodiment 12 for the first time
Method of 10700 materials to Cr in water (VI) circulation absorption
Itself the following steps are included:
(1) the WPC-0.5E-0.02C-10700 material for having adsorbed Cr (VI) in embodiment 12 for the first time is added to 1 mol/L's
In HNO3 solution, 12 h of mechanical stirring, then rinsed with deionized water to neutrality, desorption is completed in vacuum drying.
(2) Cr (VI) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is shifted after adjusting its pH=2.0
Into 50 mL conical flasks.
(3) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 35 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.
And so on, complete the third of WPC-0.5E-0.02C-10700 material in embodiment 3, the 4th and the 5th suction
It is attached.Through 5 circulation absorptions, adsorbance still reaches 75.7 mg/g.
Embodiment 14: this example is provided using the BPC-0.3U-0.05C-2500 material in embodiment 5 to Cd in water (II)
The method adsorbed for the first time
Itself the following steps are included:
(1) Cr (VI) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is transferred to 50 after adjusting its pH=6.0
In mL conical flask.
(2) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 25 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.Experiment only needs 20 min just to reach balance, counts
Obtained equilibrium adsorption capacity is 110.1 mg/g, adsorption rate 88.1%.
Embodiment 15: this example is provided using the BPC-0.3U-0.05C- for having adsorbed Cd (II) in embodiment 14 for the first time
Method of 2500 materials to Cd in water (II) circulation absorption
Itself the following steps are included:
(1) the WPC-0.5E-0.02C-10700 material for having adsorbed Cd (II) in embodiment 14 for the first time is added to 1 mol/L's
In HNO3 solution, 12 h of mechanical stirring, then rinsed with deionized water to neutrality, desorption is completed in vacuum drying.
(2) Cd (II) solution that 25 mL contain 50 mg/L is accurately prepared with deionized water, is shifted after adjusting its pH=6.0
Into 50 mL conical flasks.
(3) 10 mg biomass carbon materials are accurately weighed to add into conical flask, then conical flask is put into 25 DEG C of constant-temperature tables
In, the filtering of 30 min caudacorias, separation material and solution are shaken under 200 rpm revolving speeds.
And so on, complete the third of BPC-0.3U-0.05C-2500 material in embodiment 5, the 4th and the 5th absorption.
Through 5 circulation absorptions, adsorbance still reaches 89.5 mg/g.
Claims (13)
1. a kind of method for the N doping multiporous biological Carbon Materials for preparing high heavy metal adsorption performance using abandoned biomass, special
Sign is comprising following steps:
(1) first pericarp (such as mangosteen skin, lemon peel, watermelon peel, banana skin, durian shell, peanut shell, semen litchi and bagasse) is dried
It is dry, then 10 mL are sequentially added dissolved with nitrogen source (urea or second two at 1 g powder is weighed after powder with crusher and ball mill grinding
Amine) aqueous solution, 5 mL are dissolved with polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) or bromination
The ethanol solution of cetrimonium (CTAB) template (0.02 ~ 0.05 g) stirs 12 h after 1 h of ultrasound；(2) by step
(1) solution, which is transferred in hydrothermal reaction kettle, to carry out hydro-thermal process and keeps certain time, be cooled to room temperature after taking-up and will mix
It is dry in vacuum oven to close object；(3) solid of step (2) is cooled to room temperature, grind into powder, then under nitrogen atmosphere
400 ~ 700 DEG C are warming up to certain heating rate, 2 h is kept, is then cooled to room temperature；(4) by sample grind into powder,
It is respectively washed 3 times with ethyl alcohol and water, is then dried in vacuo again, obtain the N doping biological carbon materials of high absorption property.
2. the biomass carbon material that this technology is invented is used for the various heavy in adsorbed water body comprising following steps:
(1) 25 mL are accurately prepared with deionized water contains 50 mg/L heavy metal ion (Pb [II], Cu [II], Cr [VI] or Cd
[II]) solution, be transferred in 50 mL conical flasks after adjusting its pH；(2) accurately weigh 10 mg biomass carbon materials add to
In conical flask, then conical flask is put into constant-temperature table (15,25 or 35 DEG C of temperature), shakes 30 min under 200 rpm revolving speeds
Caudacoria filtering, separation material and solution.
3. the material after separation is needed by desorption and is adsorbed again to investigate it and recycle effect comprising following steps:
(1) material that will filter out is added in stripping liquid, 12 h of mechanical stirring, then is rinsed with deionized water to neutrality, vacuum
It is dry, complete desorption；(2) accurately prepared with deionized water 25 mL contain 50 mg/L heavy metal ion (Pb [II], Cu [II],
Cr [VI] or Cd [II]) solution, it is consistent with the pH value of solution of first adsorption experiment to adjust its pH() after be transferred to 50 mL conical flasks
In；(3) 10 mg materials are accurately weighed to add into conical flask, then conical flask is put into constant-temperature table, under 200 rpm revolving speeds
Shake the filtering of 30 min caudacorias, separation material and solution.
4. the method according to claim 1, wherein the quality of nitrogen source is 0.2 ~ 0.5 g in step (1).
5. the method according to claim 1, wherein the quality of template is 0.02 ~ 0.05 g in step (1).
6. the method according to claim 1, wherein the hydrothermal temperature of step (2) be 120 ~ 180 DEG C, when
Between 4 ~ 12 h.
7. the method according to claim 1, wherein heating rate is 2 ~ 10 DEG C/min in step (3).
8. the method according to claim 1, wherein pyrolysis temperature is 400 ~ 700 DEG C in step (3).
9. a kind of N doping multiporous biological matter Carbon Materials that method as claimed in one of claims 1-6 obtains.
10. according to the method described in claim 2, it is characterized in that, the pH for adjusting solution in step (1) is 2.0 ~ 8.0.
11. according to the method described in claim 2, it is characterized in that, the setting temperature of constant-temperature table is 15,25 in step (2)
Or 35 DEG C differed, but not limited to this temperature.
12. according to the method described in claim 3, it is characterized in that, the HNO that the strippant in step (1) is 1 mol/L3Solution
Or 2 mol/L Na2CO3Solution.
13. according to the method described in claim 3, it is characterized in that, in step (2) pH of solution and first adsorption experiment it is molten
Liquid pH is consistent.
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