CN106732361A - A kind of preparation method of the sludge base charcoal of the paper powder that adulterates - Google Patents

A kind of preparation method of the sludge base charcoal of the paper powder that adulterates Download PDF

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Publication number
CN106732361A
CN106732361A CN201611190533.6A CN201611190533A CN106732361A CN 106732361 A CN106732361 A CN 106732361A CN 201611190533 A CN201611190533 A CN 201611190533A CN 106732361 A CN106732361 A CN 106732361A
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China
Prior art keywords
sludge
paper
powder
charcoal
base charcoal
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CN201611190533.6A
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Chinese (zh)
Inventor
刘常青
江娟
郑育毅
刘文伟
吴春山
王菲凤
赵由才
李家兵
孙启元
谢蓉蓉
汪清环
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Fujian Normal University
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Fujian Normal University
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Priority to CN201611190533.6A priority Critical patent/CN106732361A/en
Publication of CN106732361A publication Critical patent/CN106732361A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10BDESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B53/00Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
    • C10B53/07Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of solid raw materials consisting of synthetic polymeric materials, e.g. tyres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock
    • Y02P20/143Feedstock the feedstock being recycled material, e.g. plastics
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/40Valorisation of by-products of wastewater, sewage or sludge processing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention relates to a kind of sludge base charcoal, more particularly to a kind of sludge base charcoal preparation method of the paper powder that adulterates.The method is put into baking oven and dries to constant weight after municipal sludge is air-dried first, be crushed to 4 8mm, then ground, 200 mesh sieves excessively.Finished paper, paper product processing waste material, reclaimed waste paper turn into the powder official form for filing a lawsuit powder of 200 mesh through broken, grinding, sieving after drying.By 1~5:The sludge that will have been blended and paper powder of 1~3 weight ratio are sufficiently mixed.Material is inserted in atmosphere Muffle furnace, pyrolysis obtains thermal decomposition product.Thermal decomposition product is embathed with hydrochloric acid.Hydrochloric acid is filtered off, is filtered after solid content is soaked into 20min with deionized water, repeated 5 times, be put into oven for drying to constant weight, obtain the sludge base charcoal of doping paper powder.Present invention saves preparation cost so that sludge and waste paper are turned waste into wealth, while largely improving the quality and sewage disposal performance of sludge base charcoal.

Description

A kind of preparation method of the sludge base charcoal of the paper powder that adulterates
Technical field
The present invention relates to a kind of sludge base charcoal, more particularly to a kind of sludge base charcoal preparation side of the paper powder that adulterates Method.
Background technology
Charcoal refers to the biomass remaining material after high temperature pyrolysis under anoxic conditions.Charcoal has larger ratio Surface area and loose structure, with good absorption property, can adsorb heavy metal, the ammonia in water as sewage disposal adsorbent Nitrogen, phosphate etc..
With Development of China's Urbanization, town sewage plant construction is advanced by leaps and bounds, and municipal sludge is total as sewage disposal accessory substance Amount also drastically rises, if the mishandling secondary pollution that can cause environment.The treatment disposal of sludge has turned into current environment face The Tough questions for facing.
In municipal sludge contain a certain amount of carbon, can as the raw material for preparing charcoal, but its also because contained by sludge into Divide complexity, institute's phosphorus content is relatively low, therefore the simple charcoal quality being made of it and performance are compared with commercial biological charcoal gap very Greatly, its range of application is also limited significantly with value.
Paper powder refers to the thin fibre that finished paper, paper product processing waste material, waste paper, paper pulp or the ground reprocessing of pulpboard are formed Dimension or powder.Paper powder is mixed in sludge, the phosphorus content of sludge can be improved, the sludge base charcoal quality of preparation can be made more preferably, Absorption property is more preferably.
The present invention takes and prepares charcoal to the paper powder that adulterated in sludge, improves the absorption property of sludge base charcoal, while Realize the recycling of sludge and waste paper.
The content of the invention
Preparation method and application it is an object of the invention to provide a kind of sludge base charcoal of the paper powder that adulterates, with one kind Simple exercisable mode, improves the performance of sludge base charcoal, lifts its absorption dirt-removing power in sewage disposal application.
The purpose of the present invention is achieved by the following scheme:
1st, raw material prepares
Municipal sludge (moisture content 72-80%) is air-dried under field conditions (factors), is then placed in baking oven and is dried to constant weight in 105 DEG C, 4-8mm, then ground, 200 mesh sieves excessively are crushed to after removing the debris such as stone.Finished paper, paper product processing waste material, reclaimed waste paper shine Crushed through special equipment after dry, ground, sieved, the powder official form for filing a lawsuit powder as 200 mesh.
2nd, preparation process
(1) 1~5 is pressed:The sludge that will have been blended and paper powder of 1~3 weight ratio are sufficiently mixed, standby.
(2) the material by step (1) is inserted in atmosphere Muffle furnace, is passed through the nitrogen 15min of 100-200mL/min, after with 10- The programming rate of 20 DEG C/min is heated to 400-600 DEG C, and after stopping 2-3h, stopping is heated and is cooled to 80 DEG C of dischargings, is placed on dry Cooling obtains thermal decomposition product in dry device.
(3) the hydrochloric acid for (2) step being obtained thermal decomposition product 1M embathes 5min.
(4) step hydrochloric acid (3) is filtered off, is filtered after solid content is soaked into 20min with deionized water, deionized water is soaked and mistake Filter step is repeated 5 times, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, the final sludge base life for obtaining doping paper powder Thing charcoal.
The advantage of the invention is that:
The preparation cost of sludge base charcoal has been saved, the limitation of sludge base charcoal preparation has been overcome so that sludge Turn waste into wealth with waste paper, while largely improving the quality and sewage disposal performance of sludge base charcoal.
Specific embodiment
Embodiment 1
(1) the municipal sludge (moisture content 72%) for coming will be fetched to air-dry under field conditions (factors), baking oven is then placed in 105 DEG C Moisture is removed in baking, until taking out cooling after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm, then ground, mistake 200 Mesh sieve.Paper powder raw material is crushed through special equipment after drying, ground, sieving, the powder paper powder as 200 mesh.
(2) the sludge and paper powder that 200 eye mesh screens will be crossed press 1:It is uniform that 1 ratio respectively takes 50g blending.
(3) will (2) mix material and be put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.Nitrogen is first passed through with 200mL/min speed 15min, then starts to warm up heating, and to 400 DEG C and temperature 3h is kept with 10 DEG C/min programming rates, and closing heating system makes Temperature fall to 80 DEG C, take out material and be placed on cooling in drier and obtain high temperature pyrolysis product.
(4) after high temperature pyrolysis product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filter residue is soaked with deionized water, filtered after stirring and washing 15min, the deionized water being repeated 5 times Embathe and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, to be taken out and obtain this reality after drying cooling Apply the sludge base charcoal finished product of the doping paper powder of example preparation.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 301.1mg/g, the 245.3m for the sludge base charcoal prepared using municipal sludge2/ g brings up to 502.1mg/g, 498.6m2/g。
The application of sewage disposal:Weigh 2g steps (5) gained finished product, phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, precipitated after stirring reaction, take supernatants after precipitation and determine its corresponding water quality index, show the doping paper powder sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 53.8%, 21.9% and 95.9%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 15.7%, 5.4% and 14.8% respectively.
Municipal sludge described in the present embodiment takes from Foochow Zhen Ban sewage treatment plants.
Embodiment 2
(1) the municipal sludge (moisture content 80%) for coming will be fetched to air-dry under field conditions (factors), baking oven is then placed in 105 DEG C Moisture is removed in baking, until taking out cooling after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm, then ground, mistake 200 Mesh sieve.Paper powder raw material is crushed through special equipment after drying, ground, sieving, the powder paper powder as 200 mesh.
(2) the sludge and paper powder that 200 eye mesh screens will be crossed press 3:It is uniform that 2 ratio respectively takes 90g and 60g blending.
(3) will (2) mix material and be put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.Nitrogen is first passed through with 150mL/min speed 15min, then starts to warm up heating, and to 500 DEG C and temperature 2.5h is kept with 15 DEG C/min programming rates, closes heating system Temperature fall to 80 DEG C is allowed to, taking-up material is placed on cooling in drier and obtains high temperature pyrolysis product.
(4) after high temperature pyrolysis product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filter residue is soaked with deionized water, filtered after stirring and washing 15min, the deionized water being repeated 5 times Embathe and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, to be taken out and obtain this reality after drying cooling Apply the sludge base charcoal finished product of the doping paper powder of example preparation.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 253.7mg/g, the 205.3m for the sludge base charcoal prepared using municipal sludge2/ g brings up to 445.2mg/g, 412.3m2/g。
The application of sewage disposal:Weigh 2g steps (5) gained finished product, phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, precipitated after stirring reaction, take supernatants after precipitation and determine its corresponding water quality index, show the doping paper powder sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 48.5%, 20.8% and 93.6%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 11.1%, 4.5% and 12.9% respectively.
Municipal sludge described in the present embodiment takes from Foochow Zhen Ban sewage treatment plants.
Embodiment 3
(1) the municipal sludge (moisture content 74%) for coming will be fetched to air-dry under field conditions (factors), baking oven is then placed in 105 DEG C Moisture is removed in baking, until taking out cooling after constant weight, removes the debris such as stone cleaning, with crusher in crushing to 4-8mm, then ground, mistake 200 Mesh sieve.Paper powder raw material is crushed through special equipment after drying, ground, sieving, the powder paper powder as 200 mesh.
(2) the sludge and paper powder that 200 eye mesh screens will be crossed press 5:It is uniform that 1 ratio respectively takes 100g and 20g blending.
(3) will (2) mix material and be put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.Nitrogen is first passed through with 100mL/min speed 15min, then starts to warm up heating, and to 600 DEG C and temperature 2h is kept with 20 DEG C/min programming rates, and closing heating system makes Temperature fall to 80 DEG C, take out material and be placed on cooling in drier and obtain high temperature pyrolysis product.
(4) after high temperature pyrolysis product is cooled to room temperature, 5min is embathed with the hydrochloric acid of 1M.
(5) hydrochloric acid is filtered off, filter residue is soaked with deionized water, filtered after stirring and washing 15min, the deionized water being repeated 5 times Embathe and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, to be taken out and obtain this reality after drying cooling Apply the sludge base charcoal finished product of the doping paper powder of example preparation.
Determination of iodine value:Using the sludge base charcoal prepared by the present embodiment step, its iodine number is with specific surface area by simple 215.2mg/g, the 163.3m for the sludge base charcoal prepared using municipal sludge2/ g, brings up to 378.5mg/g, 338.3m2/g。
The application of sewage disposal:Weigh 2g steps (5) gained finished product, phosphorus-containing wastewater of the input equipped with 1L electromechanics polishing processes In, precipitated after stirring reaction, take supernatants after precipitation and determine its corresponding water quality index, show the doping paper powder sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 44.1%, 18.3% and 86.4%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 10.1%, 4.2% and 11.2% respectively.
Municipal sludge described in the present embodiment takes from Foochow Zhen Ban sewage treatment plants.

Claims (4)

1. it is a kind of adulterate paper powder sludge base charcoal preparation method, it is characterized in that:
1)Baking oven is put into after moisture content 72-80% municipal sludges are air-dried to be dried to constant weight in 105 DEG C, is broken after removing the debris such as stone It is broken to 4-8mm, then ground, 200 mesh sieves excessively;Finished paper, paper product processing waste material, reclaimed waste paper pass through broken, grinding, mistake after drying Powder official form for filing a lawsuit powder of the sieve as 200 mesh;
2)Preparation process:
(1)By 1~3:The sludge that will have been blended and paper powder of 1 weight ratio are sufficiently mixed;
(2)By step(1)Material insert and be pyrolyzed in atmosphere Muffle furnace, be passed through the nitrogen 15min of 100-200 mL/min, 400-600 DEG C is heated to the programming rate of 10-20 DEG C/min afterwards, after stopping 2-3h, stopping heats and be cooled to 80 DEG C Material, is placed on cooling in drier and obtains thermal decomposition product;
(3)By step(2)The hydrochloric acid for obtaining thermal decomposition product 1-3M embathes 5min;
(4)Filter off step(3)Hydrochloric acid, by solid content with deionized water soak 20min after filter, deionized water immersion with filtering Step is repeated 5 times, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, and the final sludge base for obtaining doping paper powder is biological Charcoal.
2. the method that a kind of percolate regulating reservoir bed mud according to claim 1 prepares charcoal, it is characterized in that institute That states is immersed in KOH, and the concentration of KOH is 1~3mol/L, soaks 8~24h.
3. the method that a kind of percolate regulating reservoir bed mud according to claim 1 prepares charcoal, it is characterized in that institute That states is passed through nitrogen, and flow is 100~200 mL/min, and the time for being passed through nitrogen is 15min.
4. the method that a kind of percolate regulating reservoir bed mud according to claim 1 prepares charcoal, it is characterized in that institute Described pyrolysis is stated, condition is:Progressively it is heated between 400~600 DEG C, 2~3h is stopped between this temperature.
CN201611190533.6A 2016-12-21 2016-12-21 A kind of preparation method of the sludge base charcoal of the paper powder that adulterates Pending CN106732361A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107321323A (en) * 2017-09-04 2017-11-07 四川建筑职业技术学院 A kind of sorbing material and preparation method thereof
CN107442153A (en) * 2017-08-02 2017-12-08 江苏大学 A kind of g C based on the modification of waste paper biomass carbon3N4The Preparation method and use of composite photo-catalyst
CN110550973A (en) * 2019-10-14 2019-12-10 福建师范大学 preparation method of sludge-based biochar-doped pig manure compost
CN111389368A (en) * 2020-04-22 2020-07-10 徐州工程学院 Preparation method of excess sludge biochar and application of excess sludge biochar in removing tetracycline in water
CN112516964A (en) * 2020-11-16 2021-03-19 湖南大学 Nitrogen-doped biochar and preparation method and application thereof
CN113578269A (en) * 2021-08-30 2021-11-02 南通大学 Waste paperboard biochar for treating rhodamine B dye wastewater and preparation method and application thereof
CN113648973A (en) * 2021-09-18 2021-11-16 沈阳大学 Preparation method of sludge-based biochar doped with mushroom bran
CN113967462A (en) * 2021-06-10 2022-01-25 南通大学 Preparation method and application of waste paperboard biochar
CN114733480A (en) * 2022-03-28 2022-07-12 上海园林绿化建设有限公司 Modified biochar and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102078791A (en) * 2011-01-05 2011-06-01 北京工业大学 Sludge activated carbon and preparation method thereof
CN104069810A (en) * 2014-07-03 2014-10-01 浙江省海洋开发研究院 Method for preparing activated charcoal from paper mill sludge and pine through co-pyrolysis
CN105498700A (en) * 2014-09-22 2016-04-20 北京大学深圳研究生院 Bagasse mixing sludge adsorbent preparation and modification method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102078791A (en) * 2011-01-05 2011-06-01 北京工业大学 Sludge activated carbon and preparation method thereof
CN104069810A (en) * 2014-07-03 2014-10-01 浙江省海洋开发研究院 Method for preparing activated charcoal from paper mill sludge and pine through co-pyrolysis
CN105498700A (en) * 2014-09-22 2016-04-20 北京大学深圳研究生院 Bagasse mixing sludge adsorbent preparation and modification method

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107442153A (en) * 2017-08-02 2017-12-08 江苏大学 A kind of g C based on the modification of waste paper biomass carbon3N4The Preparation method and use of composite photo-catalyst
CN107321323A (en) * 2017-09-04 2017-11-07 四川建筑职业技术学院 A kind of sorbing material and preparation method thereof
CN110550973A (en) * 2019-10-14 2019-12-10 福建师范大学 preparation method of sludge-based biochar-doped pig manure compost
CN111389368A (en) * 2020-04-22 2020-07-10 徐州工程学院 Preparation method of excess sludge biochar and application of excess sludge biochar in removing tetracycline in water
CN112516964A (en) * 2020-11-16 2021-03-19 湖南大学 Nitrogen-doped biochar and preparation method and application thereof
CN113967462A (en) * 2021-06-10 2022-01-25 南通大学 Preparation method and application of waste paperboard biochar
CN113578269A (en) * 2021-08-30 2021-11-02 南通大学 Waste paperboard biochar for treating rhodamine B dye wastewater and preparation method and application thereof
CN113648973A (en) * 2021-09-18 2021-11-16 沈阳大学 Preparation method of sludge-based biochar doped with mushroom bran
CN114733480A (en) * 2022-03-28 2022-07-12 上海园林绿化建设有限公司 Modified biochar and preparation method thereof

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Application publication date: 20170531