CN106976875A - A kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal - Google Patents

A kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal Download PDF

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Publication number
CN106976875A
CN106976875A CN201710271971.3A CN201710271971A CN106976875A CN 106976875 A CN106976875 A CN 106976875A CN 201710271971 A CN201710271971 A CN 201710271971A CN 106976875 A CN106976875 A CN 106976875A
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aromatic hydrocarbon
polycyclic aromatic
base charcoal
sludge
sludge base
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CN201710271971.3A
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CN106976875B (en
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郑育毅
陈琬
江娟
刘常青
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 newruilai Agricultural Development Co., Ltd
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Fujian Normal University
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Abstract

The present invention relates to a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal.The preparation method, it is characterised in that:(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal according to polycyclic aromatic hydrocarbon elimination liquid:Sludge base charcoal=1~3:Conical flask is moved into after 1 volume ratio mixing, will be shaken in conical flask light protected environment;(2) conical flask is taken out, and suction filtration removes filtrate, leaves solid content;(3) solid content is embathed into 5min with 1M hydrochloric acid;(4) hydrochloric acid is filtered off, solid content is soaked with deionized water and filtered after 15min, deionized water immersion is repeated 3 times with filtration step, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, that is, obtains the sludge base charcoal for removing polycyclic aromatic hydrocarbon.The advantage of the invention is that:By reducing the content of polycyclic aromatic hydrocarbon in sludge base charcoal, influence of the applying sludge base charcoal to soil and environment is solved, the security risk of agricultural product is alleviated, breach the agricultural limitation of sludge base charcoal.

Description

A kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal
Technical field
The technical method of polycyclic aromatic hydrocarbon is reduced the present invention relates to a kind of, in more particularly to a kind of reduction sludge base charcoal The method of polycyclic aromatic hydrocarbon content.
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 solve the problems, such as the hardened gas permeability of soil as soil conditioner, The ability of soil fertilizer water conservation is improved, promotes plant growth.
Contain a certain amount of carbon in sludge, sludge base charcoal can be made into as the raw material for preparing charcoal, can For sewage disposal, waste gas absorption, soil improvement etc..Presently disclosed charcoal prepares base material, be more common in agricultural abandon thing with And agricultural process produce abandon thing.Simplified process is as follows:(1) discarded object is handled, obtains the powdered of drying Biomass raw material;(2) biomass raw material are inserted in anoxybiotic and logical protective gas and sealed processor, then carries out two The heating treatment in stage, the heating treatment of first stage is to be rapidly heated from normal temperature to 220 DEG C~260 DEG C, the liter of second stage Temperature is processed as rising to 350 DEG C~750 DEG C at a slow speed from the final temperature of first stage, continues oxygen barrier and cracks 1~3 hour;(3) then cooling To room temperature, the material that step (2) is obtained is obtained after sequentially passing through grinding sieving, activator activation, distillation water washing and drying Solid biologic charcoal.The preparation process of charcoal, no doubt raw material be easy to get, with low cost, process is simple, when in obtained charcoal, Remain more polycyclic aromatic hydrocarbon, such as benzo[α, a variety of polycyclic aromatic hydrocarbons such as benzo α anthracenes have carcinogenicity, once polycyclic aromatic hydrocarbon Into soil environment, great threaten is produced to crops and food security.
Although charcoal has many advantages, such as, because it is typically to be prepared by different types of discarded object, preparation The generation of polycyclic aromatic hydrocarbon, especially municipal sludge base charcoal can often be caused in pyrolytic process, this just greatly limit sludge base Charcoal application and application value.
The present invention provides the technical method that a kind of utilization root system of plant liquid removes polycyclic aromatic hydrocarbon in sludge base charcoal, makes it It is innoxious, the influence to soil and environment using charcoal is reduced, the security risk of agricultural product is alleviated.
The content of the invention
It is an object of the invention to provide a kind of simple for process, cost is low, and safe and reliable reduction sludge base life The method of polycyclic aromatic hydrocarbon content in thing charcoal, in a kind of simple exercisable mode, the polycyclic aromatic hydrocarbon of reduction sludge base charcoal contains Amount, lifting sludge base charcoal returns the safety guarantee of soil.
To realize that the technical scheme that the purpose of the present invention is used is as follows:
1st, the formula of inorganic salts nutrient solution
2nd, the preparation of root system of plant liquid
Herbal complete root system is won together with the soil being attached on root system, wet-milling in mortar is put in and obtains the plant Root system residue and residual juice, i.e. root system of plant liquid.
3rd, polycyclic aromatic hydrocarbon eliminates the preparation of liquid
Inorganic salts nutrient solution and root system of plant liquid after constant volume is pressed into root system of plant liquid:Mineral nutrition liquid=1:2~4 Polycyclic aromatic hydrocarbon, which is obtained, after volume ratio mixing eliminates liquid.
4th, the process step of polycyclic aromatic hydrocarbons in sludge
(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal according to polycyclic aromatic hydrocarbon elimination liquid:Sludge base charcoal=1~ 3:Conical flask is moved into after 1 volume ratio mixing, conical flask is placed in 30~60min of concussion in 25~35 DEG C of light protected environment, shake Swing 100-200r/min of speed;
2) conical flask is taken out, suction filtration removes filtrate, leaves solid content;
3) solid content is embathed into 5min with 1M hydrochloric acid;
4) hydrochloric acid is filtered off, solid content is soaked with deionized water and filtered after 15min, deionized water immersion and filtration step weight It is multiple 3 times, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, that is, obtain the sludge base charcoal for removing polycyclic aromatic hydrocarbon.
Herbaceous plant of the present invention is Kidney bean, pea, clover, clover or rye grass.
Sludge base charcoal preparation method of the present invention is as follows:
1) sludge (moisture content 72-80%) is air-dried under field conditions (factors), is then placed in baking oven and is dried in 105 DEG C to constant weight, Remove and 4-8mm is crushed to after the debris such as stone, then ground, 200 mesh sieves excessively obtain sludge dry powder;
2) sludge dry powder for crossing 200 mesh sieves is immersed in 8-24h in 1-3mol/L KOH, filtered filtration residue inserts baking oven Moisture is removed in 105 DEG C of bakings, until taking out cooling after constant weight;
3) by sludge dry powder insert in atmosphere Muffle furnace be pyrolyzed, be passed through 100-200mL/min nitrogen 15min, after with 10- 20 DEG C/min programming rate is heated to 400-600 DEG C, stops after 2-3h, stops heating and is cooled to 80 DEG C of dischargings, is placed on dry Cooling obtains thermal decomposition product in dry device;
4) by step 3) obtained thermal decomposition product embathes 5min with 1mol/L hydrochloric acid;
5) filter off step 4) hydrochloric acid, by solid content with deionized water soak 20min after filter, deionized water immersion and mistake Filter step to repeat 5 times, until filtrate pH is 7-8, then is put into baking oven in 105 DEG C of drying to constant weight the upper thing of filter, obtain sludge base Charcoal.
Sludge of the present invention includes the excess sludge, city river bed mud and industrial organic waste mud of sewage disposal.
The advantage of the invention is that:
1st, sludge base charcoal is handled using method of the present invention, the residual clearance of polycyclic aromatic hydrocarbon is more than 65%.
2nd, by reducing the content of polycyclic aromatic hydrocarbon in sludge base charcoal, solve applying sludge base charcoal to soil and The influence of environment, alleviates the security risk of agricultural product, breaches the agricultural limitation of sludge base charcoal.
Embodiment
Embodiment 1
1st, according to the volume content of inorganic salts in inorganic salts nutrient solution, inorganic salts nutrient solution is prepared:
2nd, root system of plant liquid
The complete root system of clover is won together with the soil being attached on root system, is put in and a small amount of water progress is added in mortar Wet-milling obtains the root system residue and residual juice of the clover, i.e. root system of plant liquid.
3rd, polycyclic aromatic hydrocarbon eliminates liquid
Inorganic salts nutrient solution and root system of plant liquid are pressed into root system of plant liquid:Mineral nutrition liquid=1:2 volume ratio mixing After obtain polycyclic aromatic hydrocarbon eliminate liquid.
4th, in sludge base charcoal polycyclic aromatic hydrocarbon processing
(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal made from sewage disposal plant excess sludge by 3:1 volume ratio Mix, move into conical flask.
(2) conical flask is placed in 30 DEG C of light protected environment and shakes 60min, concussion speed 100r/min.
(3) conical flask is taken out, and suction filtration removes filtrate, leaves solid content.
(4) hydrochloric acid is filtered off, solid content is soaked with deionized water, is filtered after stirring and washing 15min, the deionization being repeated 3 times Water logging is washed and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, the present embodiment is obtained after cooling Remove the sludge base charcoal of polycyclic aromatic hydrocarbon.
Polycyclic aromatic hydrocarbon removal effect is determined:
The sludge base charcoal that the present embodiment is used is measured containing 16 kinds of polycyclic aromatic hydrocarbons, total amount 6.78mg/kg altogether;Through this reality The polycyclic aromatic hydrocarbon for applying example is eliminated after liquid processing, and its polycyclic aromatic hydrocarbon residual volume 2.25mg/kg eliminates 4.53mg/kg, clearance altogether For 66.81%.
The present embodiment sludge picks up from Foochow East water factory.
Sludge base charcoal preparation method described in the present embodiment is as follows:
1) the remaining sludge (moisture content 72-80%) of sewage treatment plant is air-dried under field conditions (factors), is then placed in baking oven Dried in 105 DEG C and arrive constant weight, removed and 4-8mm is crushed to after the debris such as stone, then ground, 200 mesh sieves excessively obtain sludge dry powder;
2) sludge dry powder is immersed in 8-24h in 1-3mol/L KOH, filtered filtration residue is inserted baking oven and gone in 105 DEG C of bakings Moisture, until taking out cooling after constant weight;
3) by sludge dry powder insert in atmosphere Muffle furnace be pyrolyzed, be passed through 100-200mL/min nitrogen 15min, after with 10- 20 DEG C/min programming rate is heated to 400-600 DEG C, stops after 2-3h, stops heating and is cooled to 80 DEG C of dischargings, is placed on dry Cooling obtains thermal decomposition product in dry device;
4) by step 3) obtained thermal decomposition product embathes 5min with 1mol/L hydrochloric acid;
5) filter off step 4) hydrochloric acid, by solid content with deionized water soak 20min after filter, deionized water immersion and mistake Filter step to repeat 5 times, until filtrate pH is 7-8, then is put into baking oven in 105 DEG C of drying to constant weight the upper thing of filter, obtain sludge base Charcoal.
Embodiment 2
1st, according to the volume content of inorganic salts in inorganic salts nutrient solution, inorganic salts nutrient solution is prepared:
2nd, root system of plant liquid
The complete root system of Kidney bean is won together with the soil being attached on root system, be put in added in mortar a small amount of water carry out it is wet Mill obtains the root system residue and residual juice of the Kidney bean, i.e. root system of plant liquid.
3rd, polycyclic aromatic hydrocarbon eliminates liquid
Inorganic salts nutrient solution and root system of plant liquid after constant volume is pressed into root system of plant liquid:Mineral nutrition liquid=1:4 body Product eliminates liquid than obtaining polycyclic aromatic hydrocarbon after mixing.
4th, in sludge base charcoal polycyclic aromatic hydrocarbon processing
(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal made from sewage disposal plant excess sludge by 2:1 volume ratio is mixed It is even, move into conical flask.
(2) conical flask is placed in 25 DEG C of light protected environment and shakes 30min, concussion speed 200r/min.
(3) conical flask is taken out, and suction filtration removes filtrate, leaves solid content.
(4) hydrochloric acid is filtered off, solid content is soaked with deionized water, is filtered after stirring and washing 15min, the deionization being repeated 3 times Water logging is washed and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, this is obtained after taking out dry cooling The sludge base charcoal of the removing polycyclic aromatic hydrocarbon of embodiment.
Polycyclic aromatic hydrocarbon removal effect is determined:
The sludge base charcoal that the present embodiment is used is measured containing 16 kinds of polycyclic aromatic hydrocarbons, total amount 6.78mg/kg altogether;Through this reality The polycyclic aromatic hydrocarbon for applying example is eliminated after liquid processing, and its polycyclic aromatic hydrocarbon residual volume 3.01mg/kg eliminates 3.77mg/kg, clearance altogether For 55.60%.
Sludge described in the present embodiment is derived from Foochow South water factory.
Sludge base charcoal preparation method described in the present embodiment is same as Example 1.
Embodiment 3
1st, according to the volume content of inorganic salts in inorganic salts nutrient solution, inorganic salts nutrient solution is prepared:
2nd, root system of plant liquid
The complete root system of clover is won together with the soil being attached on root system, be put in added in mortar a small amount of water carry out it is wet Mill obtains the root system residue and residual juice of the clover, i.e. root system of plant liquid.
3rd, polycyclic aromatic hydrocarbon eliminates liquid
Inorganic salts nutrient solution and root system of plant liquid after constant volume is pressed into root system of plant liquid:Mineral nutrition liquid=1:3 body Product eliminates liquid than obtaining polycyclic aromatic hydrocarbon after mixing.
4th, in sludge base charcoal polycyclic aromatic hydrocarbon processing
(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal made from the excess sludge of doping cow dung by 2:1 volume ratio is mixed It is even, move into conical flask.
(2) conical flask is placed in 30 DEG C of light protected environment and shakes 45min, concussion speed 150r/min.
(3) conical flask is taken out, and suction filtration removes filtrate, leaves solid content.
(4) hydrochloric acid is filtered off, solid content is soaked with deionized water, is filtered after stirring and washing 15min, the deionization being repeated 3 times Water logging is washed and filtration step.The upper thing of filter is finally put into baking oven in 105 DEG C of drying to constant weight, this is obtained after taking out dry cooling The sludge base charcoal of the removing polycyclic aromatic hydrocarbon of embodiment.
Polycyclic aromatic hydrocarbon removal effect is determined:
The sludge base charcoal that the present embodiment is used is measured containing 18 kinds of polycyclic aromatic hydrocarbons, total amount 5.77mg/kg altogether;Through this reality 1/3 polycyclic aromatic hydrocarbon for applying example is eliminated after liquid processing, and its polycyclic aromatic hydrocarbon residual volume 1.89mg/kg eliminates 3.88mg/kg, gone altogether Except rate is 67.24%.

Claims (8)

1. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal, it is characterised in that:
(1) polycyclic aromatic hydrocarbon is eliminated into liquid with sludge base charcoal according to polycyclic aromatic hydrocarbon elimination liquid:Sludge base charcoal=1~3:1 Conical flask is moved into after volume ratio mixing, will be shaken in conical flask light protected environment;
(2) conical flask is taken out, and suction filtration removes filtrate, leaves solid content;
(3) solid content is embathed into 5min with 1M hydrochloric acid;
(4) hydrochloric acid is filtered off, solid content is soaked with deionized water and filtered after 15min, deionized water immersion repeats 3 with filtration step Time, then the upper thing of filter is put into baking oven in 105 DEG C of drying to constant weight, that is, obtain the sludge base charcoal for removing polycyclic aromatic hydrocarbon.
2. the content method of polycyclic aromatic hydrocarbon in a kind of reduction sludge base charcoal according to claim 1, it is characterised in that The formula of described inorganic salts nutrient solution is:
3. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal according to claim 1, it is characterised in that Described root system of plant liquid preparation process is as follows:Herbal complete root system is won together with the soil being attached on root system, is put Wet-milling obtains the root system residue and residual juice of the plant, i.e. root system of plant liquid in mortar.
4. a kind of method for reducing polycyclic aromatic hydrocarbon in sludge base charcoal according to claim 1, it is characterised in that described Polycyclic aromatic hydrocarbon eliminate liquid preparation process it is as follows:Inorganic salts nutrient solution and root system of plant liquid are pressed into root system of plant liquid:Inorganic salts are sought Nutrient solution=1:Polycyclic aromatic hydrocarbon, which is obtained, after 2~4 volume ratio mixing eliminates liquid.
5. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal according to claim 1, it is characterised in that Shaken in described light protected environment, oscillation environment temperature is 25~35 DEG C, concussion 30~60min of time, concussion speed 100- 200r/min。
6. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal according to claim 3, it is characterised in that Described herbaceous plant is Kidney bean, pea, clover, clover or rye grass.
7. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal according to claim 1, it is characterised in that Described sludge base charcoal refers to the biology prepared using adulterated in sludge or sludge other biomass, organic waste Charcoal.
8. a kind of method for reducing polycyclic aromatic hydrocarbon content in sludge base charcoal according to claim 7, it is characterised in that Described sludge refers to the excess sludge of sewage disposal, city river bed mud and industrial organic waste mud.
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