CN106277166B - A method of utilizing antibiotic in modification biological charcoal removal breeding wastewater - Google Patents
A method of utilizing antibiotic in modification biological charcoal removal breeding wastewater Download PDFInfo
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of methods using antibiotic in modification biological charcoal removal breeding wastewater, modification biological charcoal is obtained after air-dried biomass is broken, pyrolysis, magnesium ion modification, drying, modification biological charcoal is shaken 5-20 hours under constant temperature after mixing with the breeding wastewater after preliminary sedimentation, to the removal efficiency of antibiotic therein up to 90% or more；The method of the present invention is simple and practical, it is significant to the removal effect of pollutant, reduce influence of the breeding wastewater to environment, modified biomass preparation method used in the present invention is simple and feasible, and biomass used is cheap and easy to get, it is from a wealth of sources, biomass has also efficiently been recycled while controlling water pollution, there is good practical value and application prospect.
Description
Technical field
The present invention relates to the utilization fields of sewage disposal technology and biomass, and in particular to a kind of to be gone using modification biological charcoal
Except the method for antibiotic in breeding wastewater.
Technical background
In recent decades, in order to meet the needs of people are growing to animal products, the livestock and poultry cultivation mode in China by
Initial free-ranging is gradually converted into intensive, large-scale cultivation, and livestock and poultry breeding industry has obtained unprecedented development, still, swift and violent to send out
A large amount of waste water that the livestock and poultry breeding industry of exhibition generates become the emerging pollution sources of big and medium-sized cities and after industrial wastewater, sanitary sewage
The third-largest pollution sources afterwards, the livestock breeding wastewater that China is discharged every year are more than 10,000,000,000 tons, considerably beyond national industrial wastewater and
The summation of sanitary wastewater discharge amount.
During intensive, scale livestock and poultry cultivation, in order to prevent and control disease, it is ensured that growth of animals or poultry and volume increase
Weight gain, a large amount of antibiotic medicines are fed to animal as veterinary drug or feed addictive, China's about 6000 tons of antibiosis every year
Element is added in livestock and poultry breeding industry feed, mainly including Tetracyclines, sulfamido and quinolone antibiotics, still, absolutely
Most of antibiotic cannot be absorbed by organisms completely, wherein about 30%-90% is after kidney filtration with the shape of the original or metabolite
Formula is excreted with urine, causes the antibiotic content in livestock breeding wastewater excessively high, then result in a large amount of antibiotic into
Enter into environment, they can generate harm to different kind organism in agricultural land soil, earth's surface and underground water and the ecosystem, finally can also
It is transmitted by food chain, threatens human health.
Summary of the invention
Aiming at the problem that containing a large amount of antibiotic in breeding wastewater, the present invention is provided a kind of removed using modification biological charcoal and supported
Grow the method for antibiotic in waste water, the specific steps are as follows:
(1) air-dried biomass is crushed and is sieved；
(2) product of step (1) is pyrolyzed under inert gas protection, obtains charcoal, charcoal is ground, mistake
100 meshes；
(3) charcoal powder that step (2) obtains is that 1 ︰ 10-50 g/mL is mixed according to mass volume ratio with magnesium salt solution,
And by mixture ultrasound 0.5-1h, wherein the concentration of magnesium salt solution is 0.1-1.0mol/L；
(4) after the mixture that step (3) ultrasound is crossed shakes 2-3h in shaking table, filter cake is dried, is obtained by precipitating, filtering
Modification biological charcoal；
(5) breeding wastewater is carried out to preliminary sedimentation in sedimentation basin, removes particle and suspended matter in waste water；
(6) breeding wastewater that the modification biological charcoal that step (4) obtains was precipitated with step (5) is according to mass volume ratio
1 ︰ 100-200g/mL is mixed, after stirring 5-20h under constant temperature, the content of antibiotic in detection water outlet.
Preferably, biomass described in step (1) is highland barley stalk, rape stalk or cow dung.
Preferably, the biological particles partial size in step (1) after sieving is 0.1-0.5 cm.
Preferably, inert gas described in step (2) is nitrogen or argon gas.
Preferably, pyrolytic process described in step (2) are as follows: be warming up to 300-700 DEG C with the heating rate of 3-10 DEG C/min
After keep constant temperature, pyrolysis total duration is 3-4 h.
Preferably, magnesium salts is magnesium chloride, magnesium sulfate, magnesium nitrate or magnesium acetate in step (3).
Preferably, step (6) thermostat temperature is 20-25 DEG C.
The antibiotic contained in breeding wastewater includes one of Tetracyclines, sulfamido, quinolone antibiotics or several
Kind.
Beneficial effects of the present invention:
(1) present invention is using biomass collections such as highland barley stalk, rape stalk or cow dungs as raw material, it is from a wealth of sources, be easy to get,
It is cheap, efficiently recycle discarded biomass.
(2) modification biological charcoal prepared by has very strong stability and adsorptivity, has the function for withholding pollutant well
With with huge potentiality on pollution amelioration and control.
(3) biomass is prepared into modification biological charcoal and is used to remove antibiotic in breeding wastewater, treatment process by the present invention
Process is short, operation is succinct, and low production cost, is suitable for industrialized production, has in terms of handling breeding wastewater good
Application prospect.
Specific embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
The method of antibiotic in modification biological charcoal removal breeding wastewater is utilized described in the present embodiment, the specific steps are as follows:
(1) air-dried highland barley stalk is crushed and is sieved, the particle after sieving is 0.1-0.5cm；
(2) highland barley stalk after step (1) sieving is fitted into the small can of stainless steel with a lid and keeps certain and dredged
Looseness, after being then warming up to 700 DEG C under nitrogen protection with programmable atmosphere protection batch-type furnace with the heating rate of 10 DEG C/min
Constant temperature is kept, pyrolysis total duration is 4 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to quality with volume ratio for 1 ︰ 10g/mL, and
By mixture ultrasound 0.5h, wherein the concentration of magnesium salt solution is 0.1mol/L, magnesium salts MgCl2·6H2O；
(4) after the mixture that step (3) ultrasound is crossed shakes 3h in shaking table, filter cake is dried, is changed by precipitating, filtering
Property charcoal；
(5) compound concentration is 10ppm respectively tetracycline, sulfamethazine solution and Norfloxacin solution,
The modification biological charcoal that step (4) obtains is mixed with 3 kinds of analog culture waste water according to 1 ︰ 200g/mL, 20 DEG C of stirring 10h of constant temperature
Afterwards, the content for detecting antibiotic in water outlet, as a result see the table below 1.
Modification biological charcoal removes the effect of TC, SM2 and NOF antibiotic in analog culture waste water in 1 embodiment 1 of table
As known from Table 1, the effect of 1 gained modification biological charcoal of embodiment removal antibiotic is fine, and removal rate is 91% or more.
Embodiment 2
The method of antibiotic in modification biological charcoal removal breeding wastewater is utilized described in the present embodiment, the specific steps are as follows:
(1) air-dried rape stalk is crushed and is sieved, the particle after sieving is 0.2-0.5cm；
(2) rape stalk after step (1) sieving is fitted into the small can of stainless steel with a lid and keeps certain and dredged
Looseness is protected after being then warming up to 500 DEG C under nitrogen protection with programmable atmosphere protection batch-type furnace with the heating rate of 5 DEG C/min
Constant temperature is held, pyrolysis total duration is 4 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 40g/mL, and will
Mixture ultrasound 0.8h, wherein the concentration of magnesium salt solution is 1mol/L, and magnesium salts is magnesium acetate；
(4) after the mixture that step (3) ultrasound is crossed shakes 2h in shaking table, filter cake is dried, is changed by precipitating, filtering
Property charcoal；
(5) compound concentration is 10ppm respectively tetracycline, sulfamethazine solution and Norfloxacin solution,
The modification biological charcoal that step (4) obtains is mixed with 3 kinds of analog culture waste water according to 1 ︰ 180g/mL, 25 DEG C of stirring 15h of constant temperature
Afterwards, the content for detecting antibiotic in water outlet, as a result see the table below 2.
Modification biological charcoal removes the effect of TC, SM2 and NOF antibiotic in analog culture waste water in 2 embodiment 2 of table
As known from Table 2, the effect of 2 gained modification biological charcoal of embodiment removal antibiotic reaches 98% or more.
Embodiment 3
The method of antibiotic in modification biological charcoal removal breeding wastewater is utilized described in the present embodiment, the specific steps are as follows:
(1) air-dried cow dung is crushed and is sieved, the particle after sieving is 0.1-0.4 cm；
(2) cow dung after step (1) sieving is fitted into the small can of stainless steel with a lid and is kept certain gas porosity,
Then it is kept after being warming up to 300 DEG C under nitrogen protection with programmable atmosphere protection batch-type furnace with the heating rate of 3 DEG C/min permanent
Temperature, pyrolysis total duration are 3 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 50g/mL, and will
Mixture ultrasound 1h, wherein the concentration of magnesium salt solution is 0.5mol/L, and magnesium salts is magnesium nitrate；
(4) after the mixture that step (3) ultrasound is crossed shakes 2.5h in shaking table, filter cake is dried, is obtained by precipitating, filtering
Modification biological charcoal；
(5) it prepares tetracycline and blood concentration norfloxacin is the composite waste of 10 ppm, the modified life that step (4) is obtained
Object charcoal is mixed with analog culture waste water according to 1 ︰ 150g/mL, after 22 DEG C of stirring 5h of constant temperature, the content of antibiotic in detection water outlet,
As a result 3 be see the table below.
Modification biological charcoal removes the removal effect of Multiple Classes of Antibiotics in analog culture waste water simultaneously in 3 embodiment 3 of table
As known from Table 3, the effect of 3 gained modification biological charcoal of embodiment removal antibiotic is fine, reaches 92% or more.
Embodiment 4
The method of antibiotic in modification biological charcoal removal breeding wastewater is utilized described in the present embodiment, the specific steps are as follows:
(1) air-dried rape stalk is crushed and is sieved, the particle after sieving is 0.1-0.5cm；
(2) rape stalk after step (1) sieving is fitted into the small can of stainless steel with a lid and keeps certain and dredged
Looseness is protected after being then warming up to 600 DEG C under protection of argon gas with programmable atmosphere protection batch-type furnace with the heating rate of 6 DEG C/min
Constant temperature is held, pyrolysis total duration is 3.5 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 30g/mL, and will
Mixture ultrasound 1h, wherein the concentration of magnesium salt solution is 0.9mol/L, and magnesium salts is magnesium sulfate；
(4) after the mixture that step (3) ultrasound is crossed shakes 2.5h in shaking table, filter cake is dried, is obtained by precipitating, filtering
Modification biological charcoal；
(5) composite waste that tetracycline, sulfamethazine and blood concentration norfloxacin are 10ppm is prepared, by step
(4) the modification biological charcoal and analog culture waste water obtained is mixed according to the ratio of 1 ︰ 100g/mL, after 24 DEG C of stirring 16h of constant temperature, inspection
The content for measuring antibiotic in water, as a result see the table below 4.
Modification biological charcoal removes the removal effect of Multiple Classes of Antibiotics in analog culture waste water simultaneously in 4 embodiment 4 of table
As known from Table 4, the effect of 4 gained modification biological charcoal of embodiment removal antibiotic is fine, up to 92% or more.
Embodiment 5
Using the method for antibiotic in modification biological charcoal removal breeding wastewater described in the present embodiment, breeding wastewater is Yunnan
The waste water of pig farm discharge, wherein antibiotic content be tetracycline 1.016ppm, sulfamethazine 1.224ppm, promise fluorine it is husky
Star 0.984ppm, the specific steps are as follows:
(1) air-dried rape stalk is crushed and is sieved, the particle after sieving is 0.1-0.5cm；
(2) rape stalk that step (1) has been crushed is fitted into the small can of stainless steel with a lid and keeps certain and dredged
Looseness is protected after being then warming up to 650 DEG C under nitrogen protection with programmable atmosphere protection batch-type furnace with the heating rate of 7 DEG C/min
Constant temperature is held, pyrolysis total duration is 3.2 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 20g/mL, and will
Mixture ultrasound 0.6h, wherein the concentration of magnesium salt solution is 0.8mol/L, and magnesium salts is magnesium sulfate；
(4) after the mixture that step (3) ultrasound is crossed shakes 2h in shaking table, filter cake is dried, is changed by precipitating, filtering
Property charcoal；
(5) breeding wastewater is staticly settled, takes upper liquid；
(6) the modification biological charcoal that step (4) obtains and the breeding wastewater that step (5) were precipitated is mixed according to 1 ︰ 140g/mL
It closes, after 23 DEG C of stirring 12h of constant temperature, the content of antibiotic in detection water outlet, tetracycline is 0.083 ppm, sulfamethazine
It is 0.091 ppm for 0.105 ppm, Norfloxacin, removal rate is respectively 91.83%, 91.42%, 90.75%.
Embodiment 6
Using the method for antibiotic in charcoal removal breeding wastewater described in the present embodiment, breeding wastewater is Yunnan poultry
The waste water of factory's discharge, wherein antibiotic content is tetracycline 1.273ppm, Norfloxacin 0.899ppm, the specific steps are as follows:
(1) air-dried highland barley stalk is crushed and is sieved, the particle after sieving is 0.1-0.5cm；
(2) highland barley stalk that step (1) has been crushed is fitted into the small can of stainless steel with a lid and keeps certain and dredged
Looseness is protected after being then warming up to 550 DEG C under nitrogen protection with programmable atmosphere protection batch-type furnace with the heating rate of 8 DEG C/min
Constant temperature is held, pyrolysis total duration is 3.8 h, and charcoal is made and sieves with 100 mesh sieve after grinding；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 35g/mL, and will
Mixture ultrasound 0.9h, wherein the concentration of magnesium salt solution is 0.4mol/L, and magnesium salts is magnesium sulfate；
(4) after the mixture that step (3) ultrasound is crossed shakes 3h in shaking table, filter cake is dried, is changed by precipitating, filtering
Property charcoal；
(5) breeding wastewater is staticly settled, takes upper liquid；
(6) the modification biological charcoal that step (4) obtains and the breeding wastewater that step (5) were precipitated is mixed according to 1 ︰ 160g/mL
It closes, after 25 DEG C of stirring 20h of constant temperature, the content of antibiotic in detection water outlet, tetracycline 0.092ppm, Norfloxacin are
0.076ppm, removal rate are respectively 92.77%, 91.54%；
Above embodiments are merely to illustrate the present invention, but protection content of the invention is not limited to the above content, not
Under the spirit and scope of inventive concept, various changes and advantages that will be apparent to those skilled in the art are all included in the present invention
It is interior.
Claims (6)
1. a kind of method using antibiotic in modification biological charcoal removal breeding wastewater, which is characterized in that specific step is as follows:
(1) air-dried biomass is crushed and is sieved；The biomass is highland barley stalk, rape stalk or cow dung；
(2) product of step (1) is pyrolyzed under inert gas protection, obtains charcoal, charcoal is ground, and crosses 100 mesh
Sieve；
(3) charcoal powder that step (2) obtains is mixed with magnesium salt solution according to mass volume ratio for 1 ︰ 10-50g/mL, and will
Mixture ultrasound 0.5-1h, wherein the concentration of magnesium salt solution is 0.1-1.0mol/L；
(4) after the mixture that step (3) ultrasound is crossed shakes 2-3h in shaking table, filter cake is dried, is modified by precipitating, filtering
Charcoal；
(5) breeding wastewater is carried out to preliminary sedimentation in sedimentation basin, removes particle and suspended matter in waste water；
(6) breeding wastewater that the modification biological charcoal that step (4) obtains was precipitated with step (5) is 1 ︰ 100- according to mass volume ratio
200g/mL is mixed, after stirring 5-20h under constant temperature, the content of antibiotic in detection water outlet.
2. utilizing the method for antibiotic in modification biological charcoal removal breeding wastewater according to claim 1, which is characterized in that step
Suddenly the biological particles partial size in (1) after sieving is 0.1-0.5 cm.
3. utilizing the method for antibiotic in modification biological charcoal removal breeding wastewater according to claim 1, which is characterized in that step
Suddenly inert gas described in (2) is nitrogen or argon gas.
4. utilizing the method for antibiotic in modification biological charcoal removal breeding wastewater according to claim 1, which is characterized in that step
Suddenly pyrolytic process described in (2) are as follows: constant temperature is kept after being warming up to 300-700 DEG C with the heating rate of 3-10 DEG C/min, pyrolysis is total
Shi Changwei 3-4 h.
5. utilizing the method for antibiotic in modification biological charcoal removal breeding wastewater according to claim 1, which is characterized in that step
Suddenly magnesium salts is magnesium chloride, magnesium sulfate, magnesium nitrate or magnesium acetate in (3).
6. utilizing the method for antibiotic in modification biological charcoal removal breeding wastewater according to claim 1, which is characterized in that step
Suddenly (6) described thermostat temperature is 20-25 DEG C.
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| "Fe/Mg负载改性竹炭去除水中的氨氮";陈靖等;《环境工程学报》;20151130;第9卷(第11期);摘要、第5188页左栏第8行至5192页左栏第2行 * |
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