CN110075797A - A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material - Google Patents

A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material Download PDF

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Publication number
CN110075797A
CN110075797A CN201910370957.8A CN201910370957A CN110075797A CN 110075797 A CN110075797 A CN 110075797A CN 201910370957 A CN201910370957 A CN 201910370957A CN 110075797 A CN110075797 A CN 110075797A
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China
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reed
chicken manure
charcoal
raw material
biological carbon
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Inventor
张燕
刘雪兰
伏春燕
李新华
董红云
阎佩佩
石天虹
魏祥法
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Poultry Research Institute Shandong Academy of Agricultural Sciences
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Poultry Research Institute Shandong Academy of Agricultural Sciences
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Priority to CN201910370957.8A priority Critical patent/CN110075797A/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
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • B01J20/28064Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
    • 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
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057Surface area, e.g. B.E.T specific surface area
    • B01J20/28066Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
    • 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
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia
    • 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
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/40Capture or disposal of greenhouse gases of CO2

Abstract

The invention discloses a kind of methods for preparing biological carbon adsorbent as raw material using reed, chicken manure.Reed and chicken manure are transformed into charcoal using pyrolysismethod using the green maturity period reed of wetland, chicken manure as primary raw material by this method, pass through activator potassium silicate and CO2Activation twice, deploys reed and chicken manure different ratio prepares charcoal, further improves specific surface area, micro pore volume of charcoal etc., improves it and adsorbs pollutant ability.The reed aerial part in maturity period absorb and store nitrogen phosphorus in wet land system ability it is most strong, and chicken manure not only nutriments such as rich Nitrogen-and Phosphorus-containing itself, it is also enriched in the complicated substance such as calcium, magnesium, iron, zinc, therefore the advantage and disadvantage of reed and chicken manure are combined to prepare charcoal, the absorption property of charcoal can not only be improved, secondary pollution caused by chemical substance is added can be weakened again, also can effectively prevent the loss of the substances such as calcium in charcoal, magnesium, iron, zinc.

Description

A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material
Technical field
The present invention relates to a kind of methods for preparing biological carbon adsorbent as raw material using reed, chicken manure, belong to wetland, agricultural solid Body waste material utilizes and water environment pollution control field.
Background technique
The substances such as Water, phosphorus are more than water body itself bearing capacity, will lead to water body and periphery ecosystem disequilibrium, In turn result in degree of water pollution deterioration.In restoration of the ecosystem water pollution technology, novel absorption material such as charcoal is answered In water pollution control.Common biological carbon feedstock has wheat stalk, rice husk, timber, grass, feces of livestock and poultry etc., also has at present The report that charcoal carries out absorption pollutant is prepared using reed straw, chicken manure.Such as 106000334 A " one of Chinese patent CN Modified reed biomass carbon of kind and its preparation method and application ", a kind of 108970583 A of CN " reed base charcoal adsorbent material Preparation method ", 105170091 A of CN " preparation and its application in Removal of Phosphorus in Wastewater of the modified reed charcoal of iron ", 108236917 A of CN " a kind of modification biological charcoal based on reed straw and the application in lead contamination " and Wang Bo et al. (Adsorption law research [J] China ring of Wang Bo, Ye Chun, Li Fayun, Qu Gan, Chen Xin the water plant charcoal to nitrate nitrogen Border is scientific, 2017,37 (1): 116-122.) be to the maximal absorptive capacity of nitrate nitrogen using the reed charcoal of hydrochloric Acid Modification 14.6661mg/g.These are preferable to the pollutants adsorption effect such as phosphorus, lead, nitrate nitrogen about the report of reed charcoal, and to ammonium State N2 adsorption ability needs to be further increased, and these patents are concentrated mainly on reed straw, that is, late fall or winter Reed, and the nitrogen phosphorus that this period reed stems and leaves etc. are absorbed and utilized be transferred to once more plant root or degradation return to soil, The dynamics for reducing secondary pollution by harvesting ground reed at this time is smaller.In addition, the charcoal of reed plant production is in environment Application in improvement is needed through addition CaCl2、MgCl2、ZnCl2、FeCl2Etc. chemical substances by load be modified, still These exogenous chemical substances are added, economic cost is not only increased, there is also metal ions to take off a possibility that negative, and cause makes it have latent Pollution risk.
In addition, some researchs in relation to chicken manure charcoal removal pollutant, as 108144580 A of Chinese patent CN is " a kind of Method and biological carbon adsorbent using the biological carbon adsorbent of fermentation poultry dung preparation ", 108786736 A of CN are " a kind of to be with chicken manure The charcoal of raw material preparation and the application in chicken house purification of waste water ", 103864169 A of CN are " a kind of to be removed using charcoal The method of herbicide in sewage ", 108326023 A of CN " method that wing pod Cassia tora and charcoal joint repair Tailings Dam ", this says Bright chicken manure is that the charcoal of raw material can effectively remove phosphorus, antibiotic, herbicide, heavy metal etc., but related chicken manure is biological at present The research of charcoal absorption ammonium nitrogen still lacks.
In order to realize wetland reed plant, safe utilization of the chicken manure in environmental protection, its negative effect to environment is reduced, originally Invention provides a kind of combination charcoal prepared using wetland reed, chicken manure as raw material, prepares environment protection biological charcoal, it is intended in order to Improve charcoal absorption ammonium nitrogen and phosphatic ability, while can Adsorption other water pollutants.
Summary of the invention
The present invention overcomes above-mentioned the deficiencies in the prior art, provide one kind using reed, chicken manure as raw material and prepare charcoal The method of adsorbent.This method is with wetland green reed (maturity period reed, at the beginning of late October or 11 months, when according to different regions Phase is different), chicken manure be that reed and chicken manure using pyrolysismethod are transformed into charcoal by primary raw material, by activator potassium silicate and CO2Activation twice, deploys reed and chicken manure different ratio prepares charcoal, further improves the specific surface of charcoal Product, micro pore volume etc. improve it and adsorb pollutant ability.The reed that the present invention is fabricated to-chicken manure charcoal has biggish Specific surface area and hydroxy functional group, adsorption capacity is strong, can adsorb heavy metal, ammonium nitrogen, nitrate nitrogen, phosphate, organic dirt Object etc. is contaminated, therefore can be used as filling substrate in the sewage disposal systems such as artificial swamp, not only improving single reed, single The performance of chicken manure charcoal can also effectively improve the ability of sewage removal pollutant.
The technical scheme is that a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure, feature It is, comprising the following steps:
1) reed pre-processes
By the fresh reed plant dissection in maturity period, water-removing is immersed in potassium silicate solution, then takes out drying, grinds It crushes;
2) it mixes
Chicken manure is air-dried and is crushed, and the reed of crushing and chicken manure are uniformly mixed according to the ratio of mass ratio 1:3~10, and Further drying at low temperature;
3) reed-chicken manure primary charcoal is prepared
In in ceramic vessel, compacting capping is placed on starvation in heating furnace and is pyrolyzed mixture after taking above-mentioned drying, 2~3h of continuous heating under the conditions of 600 ± 20 DEG C obtains reed-chicken manure primary charcoal;
4) it activates
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, be passed through CO2, in furnace Interior temperature is warming up to 600 ± 20 DEG C, 2~3h of continuous heating, and the reed after activating-chicken manure biology is made in cooled to room temperature Charcoal;After pickling, washing, drying to get arrive reed-chicken manure charcoal finished product.
Further, the dissection of step 1), segment length are 5.0~10.0cm.
Further, potassium silicate and the mass ratio of reed dry weight are 0.8~1.5:1 in step 1).
Further, the water-removing of step 1) is preferred are as follows: 105 ± 5 DEG C water-removing 20-40 minutes.
Further, the drying of step 1) and step 4) is 90~105 DEG C of drying.
Further, step 2) chicken manure was crushed to 40 meshes.
Further, the low temperature of the low temperature drying of step 2) is 60~65 DEG C.
Further, the reed of the crushing of step 3) and chicken manure mass ratio are preferably 1:6~8.
Further, the CO of step 3)2Flow velocity is 60-80ml/min.
Further, the pickling, washing of step 4) are as follows: first cleaned 2~4 times with 0.5mol/L hydrochloric acid, then clear with ultrapure water It washes 2~4 times.
The charcoal of above method preparation, yield >=48%, specific surface area >=500m2/ g, micro pore volume account for charcoal Total volume ratio is >=65%.
The beneficial effects of the present invention are:
1) the phosphorus secondary pollution of wet land system nitrogen is reduced
Present invention discover that the reed aerial part in maturity period absorb and store nitrogen phosphorus in wet land system ability it is most strong, at this time Harvesting reed plant (i.e. green plants) can effectively prevent nitrogen phosphorus and be again introduced into wet land system, also effectively weakens secondary pollution and asks Topic;
2) reed-chicken manure compounding prepares charcoal, and processing sewage effect is good
The reed aerial part in maturity period absorb and store nitrogen phosphorus in wet land system ability it is most strong, and chicken manure itself is not only The nutriments such as rich Nitrogen-and Phosphorus-containing are also enriched in the complicated substance such as calcium, magnesium, iron, zinc, therefore reed and the excellent of chicken manure is combined to lack Point prepares charcoal, can not only improve the absorption property of charcoal, and can weaken secondary pollution caused by chemical substance is added, It can effectively prevent the loss of the substances such as calcium in charcoal, magnesium, iron, zinc.Tests prove that: reed-chicken manure charcoal processing sewage effect Fruit is substantially better than single reed charcoal.
3) special preparation method improves biological carbon performance
Reed and chicken manure are transformed into biology using pyrolysismethod using wetland green reed, chicken manure as primary raw material by the present invention Charcoal passes through activator potassium silicate and CO2Activation twice, deploys reed and chicken manure different ratio prepares charcoal, further Specific surface area, the micro pore volume etc. for improving charcoal improve it and adsorb pollutant ability.
4) resource utilization
The present invention is able to achieve the resource utilization to solid waste such as wetland green plants, feces of livestock and poultry, provides to saving Source, realization circular agriculture, preserving the ecological environment is of great significance.
Specific embodiment
Reed used in the embodiment of the present invention is artificial swamp or natural bioremediation purifying plant, and chicken manure is chicken farm production Solid matter out, wherein reed is green maturity period plant of the current year by the end of October or at the beginning of 11 months, at this time reed biomass it is maximum and The nitrogen and phosphorus content highest being enriched in vivo, these charcoal raw material sources are more convenient, to realize technical solution of the present invention.Below It will be described in detail the preferred embodiments of the invention, its purpose is to which the present invention is showed more clearly, and The related technical personnel of this field will can be completely showed in interest field of the invention.
Embodiment 1:(reed and chicken manure mass ratio 1:4 prepare reed-chicken manure charcoal)
1) reed pre-processes
By fresh reed plant dissection, plant segment length is that 5.0~10.0cm is immersed in 105 DEG C of water-removing 0.5h In 1mol/L potassium silicate solution, wherein potassium silicate and the mass ratio of reed dry weight are 1:1, are dried after impregnating 12h in 90~105 DEG C For 24 hours, it grinds;
2) it mixes
Chicken manure air-dried 40 meshes, and the reed of crushing and chicken manure are uniformly mixed according to the ratio of mass ratio 1:4, and It is further dried under low temperature (60~65 DEG C);
3) reed-chicken manure primary charcoal is prepared
Take above-mentioned object in ceramic vessel, compacting capping is placed on starvation in heating furnace and is pyrolyzed, under the conditions of 600 DEG C Continuous heating 2.5h obtains reed-chicken manure primary charcoal;
4) it activates
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, with 60-80ml/min Flow velocity be passed through CO2, 600 DEG C, continuous heating 2.5h are warming up in in-furnace temperature, cooled to room temperature, after activation is made Reed-chicken manure charcoal;
And first cleaned 3 times with 0.5mol/L hydrochloric acid, then cleaned 3 times with ultrapure water, in 105 DEG C drying for 24 hours to get arrive reed Reed-chicken manure charcoal finished product is labeled as PC-BC2, yield (charcoal final product quality and production charcoal reed-chicken manure raw material Mass ratio) be 48.21%, specific surface area 518.56m2/ g, it is 65.7% that micro pore volume, which accounts for charcoal total volume ratio,.
By the PC-BC2 of obtained 0.2g and there is ammonium nitrogen, phosphatic 100ml sewage (wherein ammonium nitrogen concentration 30mg/ L, phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 34.85% to constant temperature vibration, phosphatic removal rate It is 98.62%.
Embodiment 2:(reed and chicken manure mass ratio 1:7 prepare reed-chicken manure charcoal)
1) reed pre-processes
By fresh reed plant dissection, plant segment length is that 5.0~10.0cm is immersed in 105 DEG C of water-removing 0.5h In 1mol/L potassium silicate solution, wherein potassium silicate and the mass ratio of reed dry weight are 1:1, are dried after impregnating 12h in 90~105 DEG C For 24 hours, it grinds;
2) it mixes
Chicken manure air-dried 40 meshes, and the reed of crushing and chicken manure are uniformly mixed according to the ratio of mass ratio 1:7, and It is further dried under low temperature (60~65 DEG C).
3) reed-chicken manure primary charcoal is prepared
Take above-mentioned object in ceramic vessel, compacting capping is placed on starvation in heating furnace and is pyrolyzed, under the conditions of 600 DEG C Continuous heating 2.5h obtains reed-chicken manure primary charcoal;
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, with 60-80ml/min Flow velocity be passed through CO2, 600 DEG C, continuous heating 2.5h are warming up in in-furnace temperature, cooled to room temperature, after activation is made Reed-chicken manure charcoal;
And first cleaned 3 times with 0.5mol/L hydrochloric acid, then cleaned 3 times with ultrapure water, in 105 DEG C drying for 24 hours to get arrive reed Reed-chicken manure charcoal finished product is labeled as PC-BC3, yield 54.16%, specific surface area 593.56m2/ g, micro pore volume account for Charcoal total volume ratio is 68.9%.
By the PC-BC3 of obtained 0.2g and there is ammonium nitrogen, phosphatic 100ml sewage (wherein ammonium nitrogen concentration 30mg/ L, phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 39.16% to constant temperature vibration, phosphatic removal rate It is 99.37%.
Embodiment 3:(reed and chicken manure mass ratio 1:9.5 prepare reed-chicken manure charcoal)
1) reed pre-processes
By fresh reed plant dissection, plant segment length is that 5.0~10.0cm is immersed in 105 DEG C of water-removing 0.5h During 1mol/L potassium silicate is molten, wherein potassium silicate and the mass ratio of reed dry weight are 1:1, are dried after impregnating 12h in 90~105 DEG C For 24 hours, it grinds;
2) it mixes
Chicken manure air-dried 40 meshes, and the reed of crushing and chicken manure are uniformly mixed according to the ratio of mass ratio 1:9.5, and It is further dried under low temperature (60~65 DEG C).
3) reed-chicken manure primary charcoal is prepared
Take above-mentioned object in ceramic vessel, compacting capping is placed on starvation in heating furnace and is pyrolyzed, under the conditions of 600 DEG C Continuous heating 2.5h obtains reed-chicken manure primary charcoal;
4) it activates
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, with 60-80ml/min Flow velocity be passed through CO2, 600 DEG C, continuous heating 2.5h are warming up in in-furnace temperature, cooled to room temperature, after activation is made Reed-chicken manure charcoal;
And first cleaned 3 times with 0.5mol/L hydrochloric acid, then cleaned 3 times with ultrapure water, in 105 DEG C drying for 24 hours to get arrive reed Reed-chicken manure charcoal finished product is labeled as PC-BC4, yield 52.16%, specific surface area 568.74m2/ g, micro pore volume account for Charcoal total volume ratio is 64.9%.
By the PC-BC4 of obtained 0.2g and there is ammonium nitrogen, phosphatic 100ml sewage (wherein ammonium nitrogen concentration 30mg/ L, phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 36.16% to constant temperature vibration, phosphatic removal rate It is 99.02%.
Comparative example 1:(reed and chicken manure mass ratio 1:1.5 prepare reed-chicken manure charcoal)
1) reed pre-processes
By fresh reed plant dissection, segment length is immersed in 1mol/L silicic acid in 105 DEG C of water-removing 0.5h for 5.0~10.0cm In potassium solution, wherein potassium silicate and the mass ratio of reed dry weight are 1:1, are dried in 90~105 DEG C for 24 hours after impregnating 12h, grounds travel It is broken;
2) it mixes
Chicken manure was air-dried into 40 meshes, and the reed of crushing and chicken manure were uniformly mixed according to the ratio of mass ratio 1:1.5, And it is further dried under low temperature (60~65 DEG C);
3) reed-chicken manure primary charcoal is prepared
Take above-mentioned object in ceramic vessel, compacting capping is placed on starvation in heating furnace and is pyrolyzed, under the conditions of 600 DEG C Continuous heating 2.5h obtains reed-chicken manure primary charcoal;
4) it activates
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, with flow velocity 60- 80ml/min is passed through CO2, 600 DEG C, continuous heating 2.5h are warming up in in-furnace temperature, cooled to room temperature, after activation is made Reed-chicken manure charcoal;
It is first cleaned 2~4 times with 0.5mol/L hydrochloric acid, then is cleaned 2~4 times with ultrapure water, in 105 DEG C of drying for 24 hours to get arriving Reed-chicken manure charcoal finished product is labeled as PC-BC1, yield 41.57%, specific surface area 424.81m2/ g, micro pore volume Accounting for charcoal total volume ratio is 59.4%.
By the PC-BC1 of obtained 0.2g and the ammonium nitrogen having, phosphatic 100ml sewage (wherein ammonium nitrogen concentration 30mg/L, phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 28.15% to constant temperature vibration, phosphatic to go Except rate is 95.10%.
Comparative example 2: reed charcoal
By fresh reed plant dissection, plant segment length is that 5.0~10.0cm is immersed in 105 DEG C of water-removing 0.5h In 1mol/L potassium silicate solution, wherein potassium silicate and the mass ratio of reed dry weight are 1:1, are dried after impregnating 12h in 90~105 DEG C For 24 hours, it grinds;It is further dried under low temperature (60~65 DEG C) again.Take above-mentioned object in ceramic vessel, after compacting covers It is placed in starvation in heating furnace to be pyrolyzed, continuous heating 2.5h under the conditions of 600 DEG C obtains reed primary charcoal, to primary Charcoal is cooled to room temperature, then primary charcoal is placed in vacuum tube furnace, is passed through CO with flow velocity 60-80ml/min2, In-furnace temperature is warming up to 600 DEG C, continuous heating 2.5h, and cooled to room temperature is made the reed charcoal after activating, and first uses 0.5mol/L hydrochloric acid cleans 3 times, then is cleaned 3 times with ultrapure water, in 105 DEG C of drying for 24 hours to get reed charcoal finished product is arrived, marks It is denoted as P-BC1, yield 32.68%, specific surface area 368.74m2/ g, micro pore volume account for charcoal total volume ratio and are 45.9%.By the P-BC1 of obtained 0.2g and have ammonium nitrogen, phosphatic 100ml sewage (wherein ammonium nitrogen concentration 30mg/L, Phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 23.16% to constant temperature vibration, and phosphatic removal rate is 83.56%.
Comparative example 3: potassium silicate does not impregnate preparation reed charcoal
By fresh reed plant dissection, plant segment length is that 5.0~10.0cm is ground in 105 DEG C of water-removing 0.5h, And it is further dried under low temperature (60~65 DEG C).Take above-mentioned object in ceramic vessel, compacting cover be placed in heating furnace every The pyrolysis of anoxybiotic gas, heats 2.5h under the conditions of 600 DEG C, obtains reed primary charcoal;It is cooled to room temperature to primary charcoal, then Primary charcoal is placed in vacuum tube furnace, CO is passed through with flow velocity 60-80ml/min2, 600 are warming up in in-furnace temperature DEG C, continuous heating 2.5h, cooled to room temperature, the reed charcoal after activation is made, and first cleaned with 0.5mol/L hydrochloric acid Several times, then with ultrapure water it cleans several times, in 105 DEG C of drying for 24 hours to get reed charcoal finished product is arrived, is labeled as P-BC2, Its yield is 25.46%.By the P-BC sum of obtained 0.2g containing ammonium nitrogen, (wherein ammonium nitrogen is dense phosphatic 100ml sewage Degree 30mg/L, phosphate concn 50mg/L) it is mixed, for 24 hours, ammonium nitrogen removal rate is 16.73% to constant temperature vibration, phosphatic Removal rate is 72.97%.
It can be seen that reed-chicken manure charcoal processing sewage effect better than single from example 1 above -3 and comparative example 1-3 Reed charcoal, and potassium silicate solution immersion can activate reed, improve the bioactivity of reed charcoal, reed and chicken manure matter Amount is more best than the preparation of 1:6~8 reed-chicken manure charcoal properties of product.The present invention is able to achieve to wetland green plants, animal dung The resource utilization of solid waste such as just, to economize on resources, realize circular agriculture, preserving the ecological environment is of great significance; In addition, achieving the purpose that protect realization environment with pollution treatment of giving up with sewage such as charcoal obtained processing agricultural, aquaculture, industry Shield provides strong technical guarantee.

Claims (10)

1. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure, characterized in that the following steps are included:
1) reed pre-processes
By the fresh reed plant dissection in maturity period, water-removing is immersed in potassium silicate solution, then takes out drying, grind;
2) it mixes
Chicken manure is air-dried and is crushed, and the reed of crushing and chicken manure are uniformly mixed according to the ratio of mass ratio 1:3~10, and low The lower further drying of temperature;
3) reed-chicken manure primary charcoal is prepared
Mixture after taking above-mentioned drying is in ceramic vessel, and compacting capping is placed on starvation in heating furnace and is pyrolyzed, 600 2~3h of continuous heating under the conditions of ± 20 DEG C obtains reed-chicken manure primary charcoal;
4) it activates
It is cooled to room temperature to primary charcoal, then primary charcoal is placed in vacuum tube furnace, be passed through CO2, in in-furnace temperature 600 ± 20 DEG C, 2~3h of continuous heating are warming up to, reed-chicken manure charcoal after activating is made in cooled to room temperature;Through acid After washing, wash, drying to get arrive reed-chicken manure charcoal finished product.
2. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that The fresh reed plant dissection of the step 1), segment length are 5.0~10.0cm.
3. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that Potassium silicate and the mass ratio of reed dry weight are 0.8~1.5:1 in the step 1).
4. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that The water-removing of the step 1) are as follows: 105 ± 5 DEG C water-removing 20-40 minutes.
5. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that The drying of the step 1) and step 4) is 90~105 DEG C of drying;The temperature of the low temperature drying of the step 2) is 60~65 DEG C.
6. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that Step 2) the chicken manure was crushed to 40 meshes.
7. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that The reed of the crushing of the step 3) and chicken manure mass ratio are 1:6~8.
8. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that The CO of the step 3)2Flow velocity is 60-80ml/min.
9. a kind of method for preparing biological carbon adsorbent as raw material using reed, chicken manure as described in claim 1, characterized in that Pickling, the washing of the step 4) are as follows: first cleaned 2~4 times with 0.5mol/L hydrochloric acid, then cleaned 2~4 times with ultrapure water.
10. the biological carbon adsorbent of the preparation of method described in any one of claim 1-9, characterized in that its specific surface area ≥500m2/ g, it is >=65% that micro pore volume, which accounts for charcoal total volume ratio,.
CN201910370957.8A 2019-05-06 2019-05-06 A method of biological carbon adsorbent is prepared using reed, chicken manure as raw material Pending CN110075797A (en)

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