CN106698880A - Preparation method of sludge based biochar doped with hair - Google Patents

Preparation method of sludge based biochar doped with hair Download PDF

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Publication number
CN106698880A
CN106698880A CN201611190534.0A CN201611190534A CN106698880A CN 106698880 A CN106698880 A CN 106698880A CN 201611190534 A CN201611190534 A CN 201611190534A CN 106698880 A CN106698880 A CN 106698880A
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China
Prior art keywords
hair
sludge
preparation
base charcoal
based biochar
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Pending
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CN201611190534.0A
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Chinese (zh)
Inventor
刘常青
何美龙
郑育毅
刘文伟
吴春山
王菲凤
赵由才
李家兵
孙启元
谢蓉蓉
李小梅
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Fujian Normal University
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Fujian Normal University
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Priority to CN201611190534.0A priority Critical patent/CN106698880A/en
Publication of CN106698880A publication Critical patent/CN106698880A/en
Pending legal-status Critical Current

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    • 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
    • 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
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/16Total nitrogen (tkN-N)
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/18PO4-P
    • 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)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention relates to a preparation method of sludge based biochar doped with hair. The preparation method comprises steps as follows: 1, air-dried municipal sludge is put in a drying oven to be dried to constant weight, crushed, ground and screened by a 200-mesh sieve, hair is ground and sieved, and 200-mesh powder is obtained; 2, the sludge and the hair are mixed in a ratio being (1-3):1 in parts by weight; 3, a mixture is put in an atmosphere muffle furnace for pyrolysis, the temperature is increased to 400-600 DEG C after introduction of nitrogen, kept for 2-3 h and then reduced to 80 DEG C, the mixture is discharged and cooled, and a pyrolysis product is obtained; 4), the product obtained in the step 3) is subjected to immersion cleaning with hydrochloric acid for 5 min, soaked with deionized water and filtered, the step is repeated 5 times, an oversized product is put in the drying oven and dried to constant weight, and the sludge based biochar doped with the hair is obtained. With the adoption of the preparation method, the preparation cost of the sludge based biochar is reduced, limitation of preparation of the sludge based biochar is overcome, so that the sludge and the waste hair are turned into wealth, and quality and sewage treatment performance of the sludge based biochar are improved to the great extent.

Description

A kind of preparation method of the sludge base charcoal of the hair that adulterates
Technical field
The present invention relates to a kind of sludge base charcoal, more particularly to a kind of preparation of the sludge base charcoal of the hair 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.
Hair refers to human hair and pig, ox, chicken, the duck animal wool that pruning process is intended abandoning.The main component of hair It is keratoprotein, the fine powder of formation is crushed after high temperature thermal denaturation, be incorporated into sludge, the phosphorus content of sludge can be improved, can Make the sludge base charcoal quality of preparation more preferably, absorption property is more preferably.
The present invention takes and prepares charcoal to the hair that adulterated in sludge, improves the absorption property of sludge base charcoal, while Realize the recycling of sludge and hair discarded object.
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 hair 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, municipal sludge is air-dried under field conditions (factors), is then placed in baking oven and is dried to constant weight in 105 DEG C, removes the debris such as stone After be crushed to 4-8mm, then it is ground, cross 200 mesh sieves.Hair grinds after special equipment high temperature thermal denaturation, sieves, as 200 Purpose powder.
2nd, by sludge and hair according to weight portion 1~3:1 ratio is sufficiently mixed, standby.
3rd, the mixture of step (2) is inserted in atmosphere Muffle furnace and is pyrolyzed, be passed through the nitrogen 15min of 100-200mL/min, 400-600 DEG C is heated to the programming rate of 10-20 DEG C/min afterwards, after stopping 2-3h, stopping is heated and is cooled to 80 DEG C of dischargings, It is placed on cooling in drier and obtains thermal decomposition product.
4th, the product of step (3) is embathed into 5min with the hydrochloric acid of 1M.Hydrochloric acid is filtered off, solid content is soaked with deionized water Filtered after 20min, deionized water immersion is repeated 5 times with filtration step, then the upper thing of filter is put into baking oven in 105 DEG C of drying to perseverance Weight, the final sludge base charcoal for obtaining doping hair.
Hair of the present invention refers to the human hair that pruning process is intended abandoning, and pig, ox, chicken, duck etc. other move Thing fur.
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 wool hair, 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.Hair grinds after special equipment high temperature thermal denaturation, sieves, the powder as 200 mesh.
(2) the sludge and hair that 200 eye mesh screens will be crossed press 1:It is uniform that 1 ratio respectively takes 50g blending.
(3) will (2) blend homogeneous material and be put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.Nitrogen is first passed through with 200mL/min speed Gas 15min, then starts to warm up heating, and to 400 DEG C and temperature 3h is kept with 10 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.Filter off hydrochloric acid, by filter residue spend from Sub- water immersion, is filtered after stirring and washing 15min, and the deionized water being repeated 5 times is embathed and filtration step.Finally the upper thing of filter is put into In 105 DEG C of drying to constant weight, taking-up dries the sludge base biology that doping hair manufactured in the present embodiment is obtained after cooling down to baking oven Charcoal finished product.
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 501.1mg/g, 489.3m2/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 hair sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 53.9%, 22.1% and 96.7%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 15.8%, 5.6% and 15.6% respectively.
Municipal sludge described in the present embodiment is taken from:Zhen Ban sewage treatment plants of Fuzhou City.
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.Hair grinds after special equipment high temperature thermal denaturation, sieves, the powder as 200 mesh.
(2) the sludge and hair that 200 eye mesh screens will be crossed press 2:It is uniform that 1 ratio respectively takes 100g and 50g blending.
(3) (2) step is blended homogeneous material and is put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.It is first logical with 150mL/min speed Enter nitrogen 15min, then start to warm up heating, temperature 2.5h to 500 DEG C and is kept with 15 DEG C/min programming rates, close plus Hot systems are allowed to Temperature fall to 80 DEG C, and 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, filters off hydrochloric acid, by filter residue spend from Sub- water immersion, is filtered after stirring and washing 15min, and the deionized water being repeated 5 times is embathed and filtration step.Finally the upper thing of filter is put into In 105 DEG C of drying to constant weight, taking-up dries the sludge base biology that doping hair manufactured in the present embodiment is obtained after cooling down to baking oven Charcoal finished product.
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 446.6mg/g, 422.1m2/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 hair sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 49.9%, 20.6% and 93.5%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 12.5%, 4.3% and 12.8% respectively.
Municipal sludge described in the present embodiment is taken from:Zhen Ban sewage treatment plants of Fuzhou City.
Embodiment 3
(1) the municipal sludge (moisture content 75%) 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.Hair grinds after special equipment high temperature thermal denaturation, sieves, the powder as 200 mesh.
(2) the sludge and hair that 200 eye mesh screens will be crossed press 3:It is uniform that 1 ratio respectively takes 150g and 50g blending.
(3) (2) step is blended homogeneous material and is put into the treatment of atmosphere Muffle furnace high temperature pyrolysis.It is first logical with 100mL/min speed Enter nitrogen 15min, then start to warm up heating, temperature 2h to 600 DEG C and is kept with 20 DEG C/min programming rates, close heating System is allowed to Temperature fall to 80 DEG C, and 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, embathe 5min with the hydrochloric acid of 1M and (5) filter off hydrochloric acid, filter residue is spent Ionized water is soaked, and is filtered after stirring and washing 15min, and the deionized water being repeated 5 times is embathed and filtration step.Finally the upper thing of filter is put Enter baking oven in 105 DEG C of drying to constant weight, taking-up dries after cooling down the sludge base for being to obtain doping hair manufactured in the present embodiment and gives birth to Thing charcoal finished product.
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 392.6mg/g, 333.7m2/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 hair sludge of the present embodiment COD of the base charcoal to the waste waterCr, TN and TP clearances be respectively 44.3%, 18.3% and 86.1%, it is relatively simple using municipal administration The sludge base charcoal that sludge is made improves 10.2%, 4.2% and 10.9% respectively.
Municipal sludge described in the present embodiment is taken from:Zhen Ban sewage treatment plants of Fuzhou City.

Claims (4)

1. it is a kind of adulterate hair sludge base charcoal preparation method, it is characterized in that:
1)Municipal sludge is air-dried under field conditions (factors), is then placed in baking oven and is dried to constant weight in 105 DEG C, is crushed to 4-8mm, then through grinding Grind, cross 200 mesh sieves;Hair grinds after high temperature thermal denaturation, sieves, the powder as 200 mesh;
2)By sludge and hair according to weight portion 1~3:1 ratio is sufficiently mixed;
3)By step 2)Mixture insert in atmosphere Muffle furnace and be pyrolyzed, be passed through to heat up after nitrogen and be heated to 400-600 DEG C, stop After 2-3h, stopping is heated and is cooled to 80 DEG C of dischargings, is placed on cooling in drier and is obtained thermal decomposition product;
4)By step 3)Product embathe 5min with the hydrochloric acid of 1M, hydrochloric acid is filtered off, after solid content is soaked into 20min with deionized water Filtering, deionized water immersion is repeated 5 times with filtration step, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, is finally obtained Must be adulterated the sludge base charcoal of hair.
2. it is according to claim 1 it is a kind of adulterate hair sludge base charcoal preparation method, it is characterized in that described Hair refers to the human hair that pruning process is abandoned, and pig, ox, chicken, duck animal skin.
3. it is according to claim 1 it is a kind of adulterate hair sludge base charcoal preparation method, it is characterized in that described Nitrogen is passed through, throughput is 100-200 mL/min, and duration of ventilation is 15min.
4. it is according to claim 1 it is a kind of adulterate hair sludge base charcoal preparation method, it is characterized in that described Heat up heating, and programming rate is 10-20 DEG C/min.
CN201611190534.0A 2016-12-21 2016-12-21 Preparation method of sludge based biochar doped with hair Pending CN106698880A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107857245A (en) * 2017-11-01 2018-03-30 上海大学 The preparation method of high bioavilability phosphorus containing sludge base Carbon Materials
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
CN110075792A (en) * 2019-04-11 2019-08-02 兰州资源环境职业技术学院 A kind of preparation method and application based on house refuse charcoal adsorbent material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09241015A (en) * 1996-03-12 1997-09-16 Ngk Insulators Ltd Production of activated carbon from sewage sludge and device therefor
CN102078791A (en) * 2011-01-05 2011-06-01 北京工业大学 Sludge activated carbon and preparation method thereof
JP4919253B2 (en) * 2005-08-03 2012-04-18 独立行政法人産業技術総合研究所 Biological organic resource processing method and system
CN102530941A (en) * 2011-12-16 2012-07-04 北京工业大学 Sludge-based activated carbon and preparation method thereof
CN104003384A (en) * 2013-02-27 2014-08-27 上海化学工业区中法水务发展有限公司 Method for preparing activated carbon by using mixture of activated sludge and reed straws

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09241015A (en) * 1996-03-12 1997-09-16 Ngk Insulators Ltd Production of activated carbon from sewage sludge and device therefor
JP4919253B2 (en) * 2005-08-03 2012-04-18 独立行政法人産業技術総合研究所 Biological organic resource processing method and system
CN102078791A (en) * 2011-01-05 2011-06-01 北京工业大学 Sludge activated carbon and preparation method thereof
CN102530941A (en) * 2011-12-16 2012-07-04 北京工业大学 Sludge-based activated carbon and preparation method thereof
CN104003384A (en) * 2013-02-27 2014-08-27 上海化学工业区中法水务发展有限公司 Method for preparing activated carbon by using mixture of activated sludge and reed straws

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107857245A (en) * 2017-11-01 2018-03-30 上海大学 The preparation method of high bioavilability phosphorus containing sludge base Carbon Materials
CN109317098A (en) * 2018-10-25 2019-02-12 肇庆市珈旺环境技术研究院 A kind of sludge base mixed adsorbing material and preparation method thereof
CN110075792A (en) * 2019-04-11 2019-08-02 兰州资源环境职业技术学院 A kind of preparation method and application based on house refuse charcoal adsorbent material

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