CN106345407A - Preparation method of modified biochar with improved ammonia nitrogen removal ability - Google Patents
Preparation method of modified biochar with improved ammonia nitrogen removal ability Download PDFInfo
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- CN106345407A CN106345407A CN201610830642.3A CN201610830642A CN106345407A CN 106345407 A CN106345407 A CN 106345407A CN 201610830642 A CN201610830642 A CN 201610830642A CN 106345407 A CN106345407 A CN 106345407A
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- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 230000001954 sterilising effect Effects 0.000 claims abstract description 13
- 239000002028 Biomass Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000197 pyrolysis Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000003610 charcoal Substances 0.000 claims description 118
- 230000004048 modification Effects 0.000 claims description 47
- 238000012986 modification Methods 0.000 claims description 47
- 239000000203 mixture Substances 0.000 claims description 30
- 210000003608 fece Anatomy 0.000 claims description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000010257 thawing Methods 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 3
- 150000002835 noble gases Chemical class 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 1
- 238000007605 air drying Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 239000002689 soil Substances 0.000 description 6
- 239000013589 supplement Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005341 cation exchange Methods 0.000 description 2
- -1 is denoted as bc300 Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 206010002660 Anoxia Diseases 0.000 description 1
- 241000976983 Anoxia Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000007953 anoxia Effects 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood 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
- C02F1/283—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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a preparation method of modified biochar with improved ammonia nitrogen removal ability. The preparation method includes the specific steps of collecting biomass, subjecting the biomass to air drying, crushing and high-temperature pyrolysis under the protection of inert gas to obtain biochar, pulverizing the biochar prior to sieving, mixing the sieved pulverized biochar with water evenly prior to sterilization, and subjecting the sterilized biochar to circulating freezing and defreezing, suction filtration, drying and grinding so as to obtain the modified biochar. The preparation method has the advantages that the biochar is modified physically, so that the ability of the biochar to adsorb ammonia nitrogen in a water body is improved effectively, the modified biochar can be used for treatment of ammonia-nitrogen-containing wastewater, and biological and efficient utilization of the biomass is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of the modification biological charcoal improving ammonia nitrogen removal ability, belong to plateau lake ecological
Protection field.
Technical background
Nitrogen is one of important nutrient source of plant, but the nitrogen output of excess can lead to the deterioration of ecological environment, wherein ammonia
Nitrogen (nh4 +) it is one of modal nitrogen pollutant, it is mainly derived from the use of chemical fertilizer in agricultural, aquaculture, municipal sewage, wash
Wash manufacture and the mineral processing industry of agent.Ammonia nitrogen enters in the water bodys such as river, lake and can lead to body eutrophication, high concentration
Ammonia nitrogen can cause dissolved oxygen concentration in water body drastically to reduce, and aquatile and environment are done great damage.Therefore reduce soil/
In water body, the output of ammonia nitrogen is most important for quality of water environment guarantee.
Charcoal (biochar) refers under conditions of anoxia wholly or in part, by agricultural crop straw, wood materials, fowl
Animal manure just waits the slightly solubility through pyrolysis (general temperature is less than a 700 DEG C) class height aromatization produced by carbonization for the organic material solid
State material.Because charcoal has the pore structure of prosperity, and surface is rich in the oxygen-containing functional group such as-cooh ,-coh and-oh,
They produce substantial amounts of negative charges can inorganic ionss in active adsorption water or in soil (as cu2+、hg2+、nh4 +Deng) and have
Machine compound, but the effect that current charcoal is applied to remove ammonia nitrogen is bad.
Yak dung comes from highlandss, and for a long time, the yak dung of highlandss bulk deposition on grassland, to environment
Cause secondary pollution, cause the waste of resource simultaneously, the problems demand of yak dung recycling solves.Agriculturally change in recent years
Fertile use has increased the loss of Nitrogen In Soils, random discharge of domestic water etc., all may cause the eutrophy of plateau lake
Change, prepare charcoal hence with yak dung, and carry out the efficiency that physical modification improves its absorption ammonia nitrogen, reduce ammonia nitrogen in soil
Output, improve domestic water in ammonia nitrogen clearance, can effectively improve plateau eco-environment.
Content of the invention
In order to realize the recycling of garbage and the output reducing ammonia nitrogen in soil/water body, the purpose of the present invention exists
In providing a kind of preparation method of the modification biological charcoal improving ammonia nitrogen removal ability, specifically include following steps:
(1) biomass are gathered, sector-style of going forward side by side is done, and is then crushed to 0.5 ~ 3cm；
(2) in the case of being passed through inert gas shielding, the biomass high temperature pyrolysis of step (1) obtain charcoal；
(3) charcoal that step (2) is obtained pulverize, cross 100 mesh sieves after mix with water, and sterilized；
(4) the mixture circulating frozen after step (3) sterilizing is thawed and be modified；
(5) product after terminating step (4) freeze-thaw circulation carries out sucking filtration, dries, and crosses 100 mesh sieves, changed after grinding
Property charcoal.
Preferably, the described biomass of step (1) are yak dung.
Preferably, the described noble gases of step (1) are nitrogen or argon.
Preferably, the heating rate for 3 ~ 5 DEG C/min for the described pyrolytical condition of step (2) is incubated 1 after being warming up to 300 ~ 600 DEG C
~ 2.5h, furnace cooling in the case of persistently leading to noble gases.
Preferably, the described mixing with water of step (3) is that the ratio for 1:2 ~ 1:4 is mixed in mass volume ratio by charcoal with water
Close uniformly.
Preferably, the described sterilizing of step (3) be add in the charcoal after mixing with water mix after volume of mixture 1% ~
2% sodium azide solution simultaneously mixes, and wherein the concentration of sodium azide solution is 10 ~ 20 g/l, or by the life after mixing with water
Thing charcoal is heated to 121 DEG C in high temperature sterilize pot and is incubated 0.5 ~ 1 hour, natural cooling.
Preferably, the condition that the described circulating frozen of step (4) thaws is: cryogenic temperature is -80 ~ -20 DEG C, and cooling time is
7 ~ 9 hours, thaw point be 20 ~ 35 DEG C, thawing time be 15 ~ 17 hours, the cooling time in one of cycle period with
Thawing time summation is 24 hours, and in 30 ~ 60 cycles of freeze-thaw circulation, period keeps the moisture content of charcoal and aqueous mixtures
Constant.
Preferably, the described drying of step (5) is that 6 ~ 8h is dried at 100 ~ 110 DEG C.
Beneficial effects of the present invention:
(1) with highlandss yak dung as biomass material, raw material abundance is easy to get the present invention, and can effectively achieve discarded
Thing recycling, reduces the secondary pollution of yak dung；
(2) present invention provides a kind of preparation method of the modification biological charcoal improving ammonia nitrogen removal ability, and described method of modifying is thing
Reason is modified, simple, environmental protection, and can effectively improve the adsorption efficiency to ammonia nitrogen for the charcoal, thus significantly more efficient
Reduce the output of ammonia nitrogen in soil, improve the clearance of ammonia nitrogen in domestic water, there is preferable practical prospect.
Brief description
Fig. 1 be the embodiment of the present invention 1 preparation charcoal before modified sem figure；
Fig. 2 is the modified sem figure of the charcoal of the embodiment of the present invention 1 preparation；
Fig. 3 adsorbs the pseudo-second order kinetic curve of ammonia nitrogen before modified afterwards for the charcoal that the embodiment of the present invention 1 prepares.
Specific embodiment
Further describe the present invention below by specific embodiment, but be merely to illustrate and explain the present invention.
Embodiment 1
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be then crushed to 0.5 ~ 3cm；
(2) step (1) gained yak dung be passed through nitrogen protection in the case of, after the heating rate of 5 DEG C/min is warmed up to 600 DEG C
Constant temperature 60min, with stove natural cooling in the case of maintaining nitrogen purge；
(3) step (2) gained charcoal is pulverized, and crosses 100 mesh sieves, prepared standard biologic charcoal, is denoted as bc600, by charcoal and water
In the ratio mix homogeneously for 1:4 for the mass volume ratio, the concentration being subsequently adding volume of mixture 1% is that the Hydrazoic acid,sodium salt of 20g/l goes out
Bacterium, and mix；
(4) mixture after step (3) sterilizing is circulated freeze-thaw, with 24h for a cycle period, first cold at -20 DEG C
Freeze 8h, then in 35 DEG C of defrosting 16h, in 30 cycles of freeze-thaw circulation, period keeps charcoal to contain with the moisture of aqueous mixtures
Amount is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 110 DEG C
Lower drying 6h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal, be designated as pbc600.
Weigh the modification biological charcoal pbc600 0.2g of the charcoal bc600 that step (3) obtains and step (5) gained respectively
In 50ml centrifuge tube, add the nh of 20mg/l4Cl solution 20ml, mixes, vibration, in different time points sampling, crosses 0.45 μm
Filter membrane, measures nh4 +Concentration.
The physicochemical property of charcoal includes: constituent content, specific surface area, ph value, cation exchange capacity (CEC) (cec) and zeta electricity
Position, is respectively adopted elemental analyser, automatically quick specific surface area and mesopore/micropore analyser, ph meter, inductively coupled plasma
Body emission spectrometer and zeta current potential and Nano/micron Particle Size Analyzer measure, and concrete data analysiss are shown in Table 1, and in addition use is sent out
Penetrate sem observation charcoal surface morphology characteristics, result is shown in Fig. 1, Fig. 2.
Physicochemical property contrast before and after table 1 charcoal physical modification
After physical modification, c, h, o, n of charcoal increase by 2.3%, 4.9%, 1.2%, 5.1% respectively as shown in Table 1, charcoal physics
Modified specific surface area increased 2.3 times；Cation exchange capacity (CEC) increases by 75.7%；Ph value reduction by 6.7%；Zeta current potential reduces
18.1%.These results indicate that charcoal is after physical modification, charcoal specific surface area and acidic functionality all increase, favorably
Adsorb ammonia nitrogen in charcoal.
Fig. 1 is charcoal sem figure before modified, and Fig. 2 is the modified sem figure of charcoal, and as seen from the figure, charcoal is modified
Front and rear surfaces are respectively provided with more pore structure, have the physical basis of absorption ammonia nitrogen, and modified hole substantially increases.
Fig. 3 is the pseudo-second order kinetic curve of charcoal absorption ammonia nitrogen before and after physical modification, charcoal after physical modification
Equilibrium adsorption capacity increased 17.8%.
Embodiment 2
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be crushed to 0.5 ~ 3 cm；
(2) step (1) gained yak dung be passed through argon protection in the case of, the heating rate of 4 DEG C/min, be warmed up to 450 DEG C
Constant temperature 100min afterwards, burner hearth natural cooling, cooling period keeps argon open-minded；
(3) cross 100 mesh sieves, prepared standard biologic charcoal after step (2) gained charcoal is pulverized, be denoted as bc450, charcoal is carried out
Physical modification, yak dung charcoal and water are the ratio mix homogeneously of 1:3 in mass volume ratio, by the charcoal after mixing with water
It is heated to 121 DEG C of insulation 45min, then natural cooling in high temperature sterilize pot, complete to sterilize；
(4) charcoal after step (3) sterilizing is circulated freeze-thaw with the mixture of water, with 24h for a cycle period,
First freeze 7h at -30 DEG C, then in 25 DEG C of defrosting 17h, in 60 cycles of freeze-thaw circulation, period keeps charcoal to mix with water
The moisture of thing is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 105 DEG C
Lower drying 7h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal.
Weigh respectively the modification biological charcoal 0.1g of the charcoal bc450 that step (3) obtains and step (5) gained in 50ml from
In heart pipe, add the nh of 10mg/l4Cl solution 20ml, mixes, and after vibration 24h, solution crosses 0.45 μm of filter membrane, measures nh4 +Concentration,
Experimental result is: non-modified charcoal bc450 is 55.78% to the removal efficiency of ammonia nitrogen, the charcoal pair after physical modification
The removal efficiency of ammonia nitrogen is 68.32%.
Embodiment 3
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be crushed to 0.5 ~ 3 cm；
(2) step (1) gained yak dung be passed through nitrogen protection in the case of, the heating rate of 3 DEG C/min, be warmed up to 300 DEG C
Constant temperature 150min afterwards, burner hearth natural cooling, cooling period keeps nitrogen open-minded；
(3) step (2) gained charcoal is pulverized, and crosses 100 mesh sieves, prepared standard biologic charcoal, is denoted as bc300, charcoal is carried out
Physical modification, yak dung charcoal and water are the ratio mix homogeneously of 1:2 in mass volume ratio, are subsequently adding volume of mixture 2%
Concentration be 15g/l Hydrazoic acid,sodium salt sterilizing, and mix；
(4) charcoal after step (3) sterilizing is circulated freeze-thaw with the mixture of water, with 24h for a cycle period,
First freeze 8h at -80 DEG C, then in 30 DEG C of defrosting 16h, in 45 cycles of freeze-thaw circulation, period keeps charcoal to mix with water
The moisture of thing is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 100 DEG C
Lower drying 8h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal.
Weigh respectively the modification biological charcoal 0.2g of the charcoal bc300 that step (3) obtains and step (5) gained in 50ml from
In heart pipe, add the nh of 5mg/l4Cl solution 20ml, mixes, and after vibration 24h, solution crosses 0.45 μm of filter membrane, measures nh4 +Concentration,
Experimental result is: non-modified charcoal bc300 is 50.66% to the removal efficiency of ammonia nitrogen, the charcoal pair after physical modification
The removal efficiency of ammonia nitrogen is 65.75%.
Embodiment 4
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be crushed to 0.5 ~ 3 cm；
(2) step (1) gained yak dung be passed through nitrogen protection in the case of, the heating rate of 3 DEG C/min, be warmed up to 500 DEG C
Constant temperature 120min afterwards, burner hearth natural cooling, cooling period keeps nitrogen open-minded；
(3) step (2) gained charcoal is pulverized, and crosses 100 mesh sieves, prepared standard biologic charcoal, is denoted as bc500, charcoal is carried out
Physical modification, yak dung charcoal and water are the ratio mix homogeneously of 1:3.5 in mass volume ratio, are subsequently adding volume of mixture
1.5% concentration is the Hydrazoic acid,sodium salt sterilizing of 10g/l, and mixes；
(4) charcoal after step (3) sterilizing is circulated freeze-thaw with the mixture of water, with 24h for a cycle period,
First freeze 9h at -60 DEG C, then in 20 DEG C of defrosting 15h, in 40 cycles of freeze-thaw circulation, period keeps charcoal to mix with water
The moisture of thing is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 105 DEG C
Lower drying 8h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal.
Weigh respectively the modification biological charcoal 0.2g of the charcoal bc500 that step (3) obtains and step (5) gained in 50ml from
In heart pipe, add the nh of 5mg/l4Cl solution 20ml, mixes, and after vibration 24h, solution crosses 0.45 μm of filter membrane, measures nh4 +Concentration,
Experimental result is: non-modified charcoal bc500 is 53.35% to the removal efficiency of ammonia nitrogen, the charcoal pair after physical modification
The removal efficiency of ammonia nitrogen is 67.83%.
Embodiment 5
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be crushed to 0.5 ~ 3 cm；
(2) step (1) gained yak dung be passed through argon protection in the case of, the heating rate of 4 DEG C/min, be warmed up to 400 DEG C
Constant temperature 90min afterwards, burner hearth natural cooling, cooling period keeps argon open-minded；
(3) cross 100 mesh sieves, prepared standard biologic charcoal after step (2) gained charcoal is pulverized, be denoted as bc400, charcoal is carried out
Physical modification, yak dung charcoal and water are the ratio mix homogeneously of 1:3 in mass volume ratio, by the charcoal after mixing with water
It is heated to 121 DEG C of insulation 60min, then natural cooling in high temperature sterilize pot, complete to sterilize；
(4) charcoal after step (3) sterilizing is circulated freeze-thaw with the mixture of water, with 24h for a cycle period,
First freeze 7.5h at -40 DEG C, then in 25 DEG C of defrosting 16.5h, in 50 cycles of freeze-thaw circulation, period keeps charcoal and water
The moisture of mixture is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 105 DEG C
Lower drying 6h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal.
Weigh respectively the modification biological charcoal 0.1g of the charcoal bc400 that step (3) obtains and step (5) gained in 50ml from
In heart pipe, add the nh of 10mg/l4Cl solution 20ml, mixes, and after vibration 24h, solution crosses 0.45 μm of filter membrane, measures nh4 +Concentration,
Experimental result is: non-modified charcoal bc400 is 52.36% to the removal efficiency of ammonia nitrogen, the charcoal pair after physical modification
The removal efficiency of ammonia nitrogen is 68.71%.
Embodiment 6
Improve the preparation method of the modification biological charcoal of ammonia nitrogen removal ability described in the present embodiment, specifically include following steps:
(1) gather yak dung, air-dried, be crushed to 0.5 ~ 3 cm；
(2) step (1) gained yak dung be passed through argon protection in the case of, the heating rate of 5 DEG C/min, be warmed up to 550 DEG C
Constant temperature 80min afterwards, burner hearth natural cooling, cooling period keeps argon open-minded；
(3) cross 100 mesh sieves, prepared standard biologic charcoal after step (2) gained charcoal is pulverized, be denoted as bc550, charcoal is carried out
Physical modification, yak dung charcoal and water are the ratio mix homogeneously of 1:2 in mass volume ratio, by the charcoal after mixing with water
It is heated to 121 DEG C of insulation 30min, then natural cooling in high temperature sterilize pot, complete to sterilize；
(4) charcoal after step (3) sterilizing is circulated freeze-thaw with the mixture of water, with 24h for a cycle period,
First freeze 8h at -35 DEG C, then in 30 DEG C of defrosting 16h, in 55 cycles of freeze-thaw circulation, period keeps charcoal to mix with water
The moisture of thing is constant, and discovery moisture of weighing supplements water when reducing；
(5) product that step (4) freeze-thaw circulation obtains after terminating, carries out sucking filtration with qualitative filter paper and buchner funnel, 110 DEG C
Lower drying 6.5h, grinds, and crosses 100 mesh sieves, obtains modification biological charcoal.
Weigh respectively the modification biological charcoal 0.1g of the charcoal bc550 that step (3) obtains and step (5) gained in 50ml from
In heart pipe, add the nh of 10mg/l4Cl solution 20ml, mixes, and after vibration 24h, solution crosses 0.45 μm of filter membrane, measures nh4 +Concentration,
Experimental result is: non-modified charcoal bc550 is 51.25% to the removal efficiency of ammonia nitrogen, the charcoal pair after physical modification
The removal efficiency of ammonia nitrogen is 66.15%.
The foregoing is only the preferred embodiments of the present invention and it is not limited to parameter described above, all in the present invention
Spirit and principle within, any modification of being made, improvement, equal replace etc., should be included in protection scope of the present invention it
Interior.
Claims (8)
1. a kind of preparation method of the modification biological charcoal improving ammonia nitrogen removal ability is it is characterised in that specifically include following steps:
(1) biomass are gathered, sector-style of going forward side by side is done, and is then crushed to 0.5 ~ 3cm；
(2) under inert gas shielding, the biomass high temperature pyrolysis of step (1) obtain charcoal；
(3) charcoal that step (2) is obtained pulverize, cross 100 mesh sieves after mix with water, and sterilized；
(4) the mixture circulating frozen after step (3) sterilizing is thawed and be modified；
(5) product after terminating step (4) freeze-thaw circulation carries out sucking filtration, dries, and crosses 100 mesh sieves, changed after grinding
Property charcoal.
2. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(1) described biomass are yak dung.
3. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(2) described noble gases are nitrogen or argon.
4. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(2) heating rate for 3 ~ 5 DEG C/min for the described pyrolytical condition is incubated 1 ~ 2.5h after being warming up to 300 ~ 600 DEG C, is persistently leading to inertia
Furnace cooling in the case of gas.
5. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(3) described is that in mass volume ratio, the ratio for 1:2 ~ 1:4 is mixed homogeneously by charcoal and water with water mixing.
6. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(3) described sterilizing be in the charcoal after mixing with water add mix after volume of mixture 1% ~ 2% sodium azide solution simultaneously
Mix, wherein the concentration of sodium azide solution is 10 ~ 20g/l, or the charcoal after mixing with water is heated to 121 DEG C of insulations
0.5 ~ 1 hour, natural cooling.
7. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(4) condition that described circulating frozen thaws is: cryogenic temperature is -80 ~ -20 DEG C, and cooling time is 7 ~ 9 hours, and thaw point is
20 ~ 35 DEG C, thawing time is 15 ~ 17 hours, and the cooling time in one of cycle period and thawing time summation are little for 24
When, in 30 ~ 60 cycles of freeze-thaw circulation, period keeps charcoal constant with the moisture content of aqueous mixtures.
8. the preparation method of modification biological charcoal improving ammonia nitrogen removal ability according to claim 1 is it is characterised in that step
(5) described drying is that 6 ~ 8h is dried at 100 ~ 110 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555411A (en) * | 2017-07-14 | 2018-01-09 | 天津大学 | A kind of zinc-rich charcoal preparation method |
| CN108569768A (en) * | 2017-08-04 | 2018-09-25 | 东北师范大学 | A kind of method that maize straw prepares artificial swamp matrix |
| CN110227414A (en) * | 2018-03-06 | 2019-09-13 | 华南农业大学 | A kind of activation method of charcoal micropore and the application in removal water body ammonia nitrogen |
| CN110420620A (en) * | 2019-07-23 | 2019-11-08 | 贵州省贵福生态肥业有限公司 | A kind of waste edible fungus bacteria stick prepares charcoal method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR0155200B1 (en) * | 1995-08-11 | 1998-11-16 | 양경선 | A method for a lawn compost |
| CN104030862A (en) * | 2014-06-13 | 2014-09-10 | 沈阳大学 | Method for preparing cow dung charcoal for inhibiting nitrogenous fertilizer leaching loss |
| CN105921110A (en) * | 2016-06-02 | 2016-09-07 | 环境保护部华南环境科学研究所 | Preparation method and application of cow dung biological carbon |
-
2016
- 2016-09-19 CN CN201610830642.3A patent/CN106345407A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR0155200B1 (en) * | 1995-08-11 | 1998-11-16 | 양경선 | A method for a lawn compost |
| CN104030862A (en) * | 2014-06-13 | 2014-09-10 | 沈阳大学 | Method for preparing cow dung charcoal for inhibiting nitrogenous fertilizer leaching loss |
| CN105921110A (en) * | 2016-06-02 | 2016-09-07 | 环境保护部华南环境科学研究所 | Preparation method and application of cow dung biological carbon |
Non-Patent Citations (2)
| Title |
|---|
| DE-LI SU等: "THE SIMULATED EFFECTS OF FREEZING AND THAWING ON PROPERTIES AND SORPTION CHARACTERISTICS FOR CARBAMAZEPINE OF BIOCHAR", 《2015 INTERNATIONAL CONFERENCE ON ENERGY, ENVIRONMENTAL & SUSTAINABLE ECOSYSTEM DEVELOPMENT》 * |
| 林静雯等: "牛粪生物炭吸附水中ＮＨ＋４的影响因素及特性", 《沈阳大学学报（自然科学版）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555411A (en) * | 2017-07-14 | 2018-01-09 | 天津大学 | A kind of zinc-rich charcoal preparation method |
| CN108569768A (en) * | 2017-08-04 | 2018-09-25 | 东北师范大学 | A kind of method that maize straw prepares artificial swamp matrix |
| CN108569768B (en) * | 2017-08-04 | 2021-06-18 | 东北师范大学 | Method for preparing constructed wetland substrate from corn straws |
| CN110227414A (en) * | 2018-03-06 | 2019-09-13 | 华南农业大学 | A kind of activation method of charcoal micropore and the application in removal water body ammonia nitrogen |
| CN110420620A (en) * | 2019-07-23 | 2019-11-08 | 贵州省贵福生态肥业有限公司 | A kind of waste edible fungus bacteria stick prepares charcoal method |
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