CN105731752B - A method of charcoal is prepared using excess sludge and hazelnut shell copyrolysis - Google Patents

A method of charcoal is prepared using excess sludge and hazelnut shell copyrolysis Download PDF

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CN105731752B
CN105731752B CN201610275811.1A CN201610275811A CN105731752B CN 105731752 B CN105731752 B CN 105731752B CN 201610275811 A CN201610275811 A CN 201610275811A CN 105731752 B CN105731752 B CN 105731752B
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charcoal
excess sludge
hazelnut shell
pyrolysis
drying
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CN105731752A (en
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赵冰
徐新阳
陈熙
李海波
张铭川
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Northeastern University China
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    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/40—Valorisation of by-products of wastewater, sewage or sludge processing

Abstract

The present invention provides a kind of method for preparing charcoal using excess sludge and hazelnut shell copyrolysis, processing step are as follows: will be broken into 1mm solid particle below after excess sludge and hazelnut shell drying respectively；Liquor zinci chloridi is added after being mixed in a certain ratio, in impregnating for 24 hours and dry under room temperature；By the hybrid particles vacuum pyrolysis after drying；Thermal decomposition product successively uses dilute hydrochloric acid, deionized water washing, obtains charcoal after drying.Excess sludge is carried out mixed pyrolysis with the hazelnut shell containing a large amount of organic matters and prepares charcoal by the present invention, in conjunction with ZnCl2The activation pore forming method that solution impregnates makes pyrolytic process be easier to occur, and compared with the mode of the crops pyrolysis such as direct burning, pyrolysis and addition corn stover, the present invention contributes to form the good charcoal product of yield height, large specific surface area, porosity.

Description

A method of charcoal is prepared using excess sludge and hazelnut shell copyrolysis
Technical field
The invention belongs to sludge treatment technique technical fields, in particular to a kind of to utilize excess sludge and hazelnut shell copyrolysis The method for preparing charcoal.
Background technique
The sludge of sewage treatment plant's discharge is divided into five classes: primary sludge, activated sludge, corruption by processing method and separation process Grow sludge, chemical sludge and precipitating sludge.Wherein activated sludge of the excess sludge outside discharge system in secondary settling tank, has The characteristics of content of organic matter height and the carbon of enriched, carbon therein can effectively be retained by being subject to anoxybiotic pyrolysis, be turned Become minimizing, innoxious, safe during sludge treatment, and the charcoal product with economic value added, avoids simultaneously The drawbacks of preparing charcoal in traditional mode of production using wood material and consume a large amount of natural vegetations.
Charcoal is a kind of carbon content charcoal extremely abundant, almost pure carbon, and major function is embodied in following side Face: 1. carbon solidification effect: charcoal is stable carbon fixation carrier, can be that armaticity carbon skeleton be sealed in soil by unstable carbon conversion In earth, inhibit the discharge of greenhouse gases, mitigates greenhouse effects；2. soil improvement: biological carbon surface contains the plants such as nitrogen, phosphorus, potassium Nutrient needed for growing, the physicochemical property of soil can be improved by making an addition in soil；3. adsorption effect: charcoal is rich in micropore knot Structure has very strong adsorption capacity, can be used as adsorbent removal sewage, pollutant in atmosphere.
With the attention of major pollutants emission reduction engineering in economic rapid development and Environmental protection, to residue Being effectively treated to be allowed to turn waste into wealth of sludge is increasingly becoming the serious problem that environmentalists face.At present to excess sludge Processing mode mainly has following three kinds: corn stover pyrolysis is added in sludge incineration, directly pyrolysis.
Sludge incineration method is that dewatered sludge is sent directly into incinerator burning, can be complete by moisture all in sludge and organic matter Portion's removal, sludge itself become ashes, and this method is suitable for industrial sludge containing a small amount of nuisance or organic concentration is high Industrial wastewater, and the disadvantage is that needing to consume a large amount of energy, equipment requirement is high, and operational management is complicated.In addition, burning process is also The hypertoxic product dioxin for having become environment hot spot at present can be generated.
Directly pyrolysis is to heat under anaerobic to it using the thermal instability of organic matter in sludge, make organic matter Thermal cracking is generated, this method energy utilization rate is higher, and generates without the pernicious gases such as dioxin and furans, but this method is run Higher cost, and the charcoal specific surface area formed is lower, pore structure is poor, is unfavorable for developing benefit as adsorbent material etc. With.
Corn stover pyrolysis, which is added, can increase the specific surface area of charcoal, optimize pore structure, but waving in corn stover Hair part content is larger, and the mass loss in pyrolytic process is more, directly contributes the low yield of charcoal.
The available charcoal of excess sludge is handled using these three modes, but has yield universal lower, obtained The defects of charcoal specific surface area and porosity are poor, absorption property is bad, contents of heavy metal elements is higher.Therefore, it needs out The excess sludge processing method for sending out that biological carbon yield is high, performance is good and environmental-friendly a kind of.
Summary of the invention
In view of the problems of the existing technology, the present invention is provided a kind of prepared using excess sludge and hazelnut shell copyrolysis and given birth to Excess sludge is mixed according to a certain percentage with hazelnut shell, is pyrolyzed under given conditions, yield is prepared by the method for object charcoal The charcoal that height, large specific surface area, pore structure are good, heavy metal element is in residual form (immobilization).Technical solution of the present invention Are as follows:
A method of charcoal being prepared using excess sludge and hazelnut shell copyrolysis, is sequentially included the following steps:
(1) excess sludge and hazelnut shell are dried respectively；
(2) excess sludge after drying is broken into 1mm solid particle below with hazelnut shell respectively；
(3) will excess sludge and the solid particle of hazelnut shell mix after liquor zinci chloridi is added, in impregnating under room temperature For 24 hours, it dries；
(4) by the hybrid particles vacuum pyrolysis after drying；
(5) it successively uses dilute hydrochloric acid, deionized water to wash in the mixture after pyrolysis, obtains charcoal after drying.
In the above method, hazelnut shell accounts for the 5 ~ 30% of excess sludge and hazelnut shell gross mass in the step (3).
In the above method, the concentration of liquor zinci chloridi is 2 ~ 5mol/L in the step (3).
In the above method, the condition of vacuum pyrolysis in the step (4) are as follows: vacuum degree is 100 ~ 500Pa, and heating rate is 10 DEG C/min, pyrolysis final temperature is 400 ~ 700 DEG C, and the time is 15 ~ 120min.
In the above method, the temperature dried in the step (1), (3) and (5) is 100 ~ 110 DEG C, and the time is 22 ~ 26h.
In the above method, the specific surface area of the charcoal is 632.54 ~ 806.15m2/ g, iodine sorption value be 589.27 ~ 669.15mg/g。
The principle of the present invention are as follows: fibert is important one of nut tree species, and yield is higher in China northeast, contains in hazelnut shell There is carbon abundant, but often discarded as rubbish, the present invention is mixed hazelnut shell as carbon source additive and excess sludge It closes, on the one hand can increase the carbon containing ratio in raw material, on the other hand since the smashed particle dispersion of hazelnut shell is good, help Mutually assemble in reducing excess sludge, therefore can promote the generation of pyrolytic reaction, the specific surface area of charcoal can be dramatically increased, and The hole be conducive in charcoal is formed, while optimizing charcoal yield, reduces contents of heavy metal elements in raw material, it is ensured that biology The environmental safety of charcoal product.
Compared with prior art, the features of the present invention and the beneficial effect is that:
Excess sludge is carried out mixed pyrolysis with the hazelnut shell containing a large amount of organic matters and prepares charcoal by the present invention, in conjunction with ZnCl2The activation pore forming method that solution impregnates makes pyrolytic process be easier to occur, with direct burning, pyrolysis and addition corn The mode of the crops such as stalk pyrolysis is compared, and the present invention contributes to form yield height, large specific surface area, the good biology of porosity Charcoal product, and heavy metal element can be stable at its pyrolytic process and is formed by crystal structure by prepared charcoal, be prevented Only precipitation in use, immobilization effect is good, realizes excess sludge to environmentally safe harmless biological charcoal product Transformation.
Hazelnut shell, the results are shown in Table 1 for corn stover Industrial Analysis.
1 hazelnut shell of table, corn stover Industrial Analysis
Industrial Analysis Moisture Mar Fixed carbon FCd Ash content Ad Fugitive constituent Vd Lower heat value LHV
Hazelnut shell 7.22% 13.98% 4.23% 74.57% 27.82MJ/kg
Corn stover 8.24% 11.94% 3.57% 76.25% 13.37MJ/kg
Note: ar indicates As-received；D indicates butt.
Detailed description of the invention
Fig. 1 is the SEM figure using the charcoal of direct method for pyrolysis preparation；
Fig. 2 is the outside drawing of charcoal prepared by the embodiment of the present invention 1；
Fig. 3 is the SEM figure of charcoal prepared by the embodiment of the present invention 1；
Fig. 4 is the SEM figure of charcoal prepared by the embodiment of the present invention 2；
Fig. 5 is the SEM figure of charcoal prepared by the embodiment of the present invention 3.
Specific embodiment
The present invention implements the excess sludge used and comes from Liaoning sewage treatment plant, Industrial Analysis and elemental analysis difference As shown in tables 2 and 3.
2 excess sludge Industrial Analysis of table
Industrial Analysis Moisture Mar Fixed carbon FCd Ash content Ad Fugitive constituent Vd Lower heat value LHV Content of organics
Content 79.54% 1.13% 33.43% 60.34% 14.90 MJ/kg 64.73%
Note: ar indicates As-received；D indicates butt.
3 excess sludge elemental analysis of table
Element C H O N S C/H C/N TN
Content (mg/kg) 36.83% 4.813% 52.164% 5.03% 1.163% 7.6526 7.3218 2.825
Element TP TK Cu Ni Pb Zn Cd Cr
Content (mg/kg) 1.795 0.38 117.53 77.27 110.28 666.67 56.18 61.38
Following embodiment is not used to explain limiting the scope of the invention for illustrating the present invention.
In the examples below, charcoal yield is defined as:
Iodine sorption value is defined as: according to National Standard Method, " GB/T12496.8-1999 wood activated charcoal test method: iodine is adsorbed The measuring method of value ", the development degree and charcoal that characterization charcoal is greater than 1.0nm micropore are to small molecular weight impurity adsorption capacity Performance, and the specific surface area of indirect measure adsorbent.
Heavy metal element immobilization ratio is defined as: according to the standardization of European Union (BCR) species of heavy metals in soil point Grade continuous extraction, in the ratio of the heavy metal element of residual form in the charcoal determined.
Inventor refers to existing direct method for pyrolysis, handles same excess sludge of the present invention:
Excess sludge is broken into 1mm solid particle below in 105 DEG C of heating afterwards for 24 hours, is 100Pa, temperature in vacuum degree Degree is vacuum pyrolysis 1h under conditions of 500 DEG C；Solid particle after being successively pyrolyzed using dilute hydrochloric acid, deionized water washing, 105 DEG C For 24 hours, obtaining charcoal yield is 45.70%, specific surface area 90.35m for drying2/ g, iodine sorption value 78.26mg/g, heavy metal Immobilization ratio are as follows: Cu, 85.22%；Ni, 83.27%；Cr, 60.81%；Cd, 71.45%；Zn, 87.36%；Pb, 76.20%.Fig. 1 The SEM figure of the charcoal of direct pyrolysis method preparation is provided, as can be seen from the figure the pattern of charcoal is in uneven gully State, but formed without nanoscale micropore, pore structure is poor, directly results in that specific surface area is low, and absorption property function is weak.
Embodiment 1
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 10% proportion excess sludge and hazelnut shell in the mixture, by the ZnCl of 5mol/L2 Solution is 2:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the hybrid particles after drying with The rate vacuum of 10 DEG C/min is heated to 500 DEG C and keeps the temperature 1.5h；Mixture after pyrolysis is successively used into dilute hydrochloric acid, deionization Water washing obtains charcoal, yield 60.49% after drying at 100 ~ 110 DEG C.In terms of absorption property: specific surface area is 799.11m2/ g, iodine sorption value 669.15mg/g；Immobilization of heavy metals ratio are as follows: Cu, 89.44%；Ni, 86.93%；Cr, 62.76%；Cd, 74.90%；Zn, 87.48%；Pb, 81.06%.Fig. 2 provides the appearance of the charcoal of the preparation of the embodiment of the present invention 1 Figure, solid particle uniform and delicate is glossy, and appearance is good, free from extraneous odour；Fig. 3 provides the SEM of charcoal manufactured in the present embodiment Figure, as can be seen from the figure the pattern of charcoal has apparent pore structure, based on micron, Nano grade hole, pore-creating compared with Deep, the more direct method for pyrolysis of specific surface area greatly improves.
Embodiment 2
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 20% proportion excess sludge and hazelnut shell in the mixture, by the ZnCl of 3mol/L2 Solution is 3:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the hybrid particles after drying with The rate vacuum of 10 DEG C/min is heated to 600 DEG C and keeps the temperature 30min；By the mixture after pyrolysis successively use dilute hydrochloric acid, go from Sub- water washing obtains charcoal, yield 56.33% after drying at 100 ~ 110 DEG C.In terms of absorption property: specific surface area is 806.15m2/ g, iodine sorption value 619.69mg/g；Immobilization of heavy metals ratio are as follows: Cu, 91.10%；Ni, 88.64%；Cr, 68.07%；Cd, 77.20%；Zn, 89.69%；Pb, 84.12%.Fig. 4 provides the SEM figure of charcoal manufactured in the present embodiment, from It can be seen that the pattern of charcoal has apparent pore structure in figure, based on micron, Nano grade hole, hole uniformly divides Cloth, the more direct method for pyrolysis of specific surface area greatly improve.
Embodiment 3
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 30% proportion excess sludge and hazelnut shell in the mixture, by the ZnCl of 4mol/L2 Solution is 3:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the hybrid particles after drying with The rate vacuum of 10 DEG C/min is heated to 400 DEG C and keeps the temperature 2h；Mixture after pyrolysis is successively used into dilute hydrochloric acid, deionized water It washs, obtains charcoal, yield 64.77% after drying at 100 ~ 110 DEG C.In terms of absorption property: specific surface area is 645.39m2/ g, iodine sorption value 652.56mg/g；Immobilization of heavy metals ratio are as follows: Cu, 89.14%；Ni, 85.08%；Cr, 63.01%；Cd, 75.23%；Zn, 88.61%；Pb, 80.32%.Fig. 5 provides the SEM figure of charcoal manufactured in the present embodiment, from It can be seen that the pattern of charcoal has apparent pore structure in figure, based on micron, Nano grade hole, pore-creating is deeper, hole Gap is evenly distributed, and the more direct method for pyrolysis of specific surface area greatly improves.
Embodiment 4
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 5% proportion excess sludge and hazelnut shell in the mixture, by the ZnCl of 2mol/L2It is molten Liquid is 3.5:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the hybrid particles after drying with The rate vacuum of 10 DEG C/min is heated to 700 DEG C and keeps the temperature 1h；Mixture after pyrolysis is successively used into dilute hydrochloric acid, deionized water It washs, obtains charcoal, yield 51.73% after drying at 100 ~ 110 DEG C.In terms of absorption property: specific surface area is 632.54m2/ g, iodine sorption value 589.27mg/g；Immobilization of heavy metals ratio are as follows: Cu, 93.44%；Ni, 88.02%；Cr, 63.62%；Cd, 77.22%；Zn, 89.27%；Pb, 83.62%.
Embodiment 5
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 15% proportion excess sludge and hazelnut shell in the mixture, by the ZnCl of 3mol/L2 Solution is 3:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the hybrid particles after drying with The rate vacuum of 10 DEG C/min is heated to 650 DEG C and keeps the temperature 1h；Mixture after pyrolysis is successively used into dilute hydrochloric acid, deionized water It washs, obtains charcoal, yield 54.30% after drying at 100 ~ 110 DEG C.In terms of absorption property: specific surface area is 751.35m2/ g, iodine sorption value 607.85mg/g；Immobilization of heavy metals ratio are as follows: Cu, 92.14%；Ni, 89.42%；Cr, 67.67%；Cd, 78.12%；Zn, 90.66%；Pb, 85.32%.
Embodiment 6
1mm solid below is broken into after respectively drying excess sludge and hazelnut shell 24 hours at 100 ~ 110 DEG C Grain；According to hazelnut shell, weight percent is 25% proportion excess sludge and hazelnut shell in the mixture, by 2.5mol/L's ZnCl2Solution is 3:1 in impregnating activation for 24 hours under room temperature with liquid-solid ratio, is dried at 100 ~ 110 DEG C；By the mixing after drying Particle is heated to 450 DEG C with the rate vacuum of 10 DEG C/min and keeps the temperature 0.75h；Mixture after pyrolysis is successively used into dilute salt Acid, deionized water are washed, and obtain charcoal, yield 61.67% after drying at 100 ~ 110 DEG C.In terms of absorption property: comparing table Area is 789.19m2/ g, iodine sorption value 659.89g/mg；Immobilization of heavy metals ratio are as follows: Cu, 88.74%；Ni, 85.14%； Cr, 64.39%；Cd, 76.49%；Zn, 89.61%；Pb, 84.33%.

Claims (3)

1. a kind of method for preparing charcoal using excess sludge and hazelnut shell copyrolysis, it is characterised in that according to the following steps into Row:
(1) excess sludge and hazelnut shell are dried respectively；
(2) excess sludge after drying is broken into 1mm solid particle below with hazelnut shell respectively；
(3) will excess sludge and the solid particle of hazelnut shell mix after liquor zinci chloridi is added, in impregnating under room temperature for 24 hours, Drying；Wherein hazelnut shell accounts for the 5~30% of excess sludge and hazelnut shell gross mass；
(4) by the hybrid particles vacuum pyrolysis after drying, the condition of the vacuum pyrolysis are as follows: vacuum degree is 100~500Pa, Heating rate is 10 DEG C/min, and pyrolysis final temperature is 400~500 DEG C, and the time is 15~120min；
(5) it successively uses dilute hydrochloric acid, deionized water to wash in the mixture after pyrolysis, charcoal, the biology is obtained after drying The specific surface area of charcoal is 632.54~806.15m2/ g, iodine sorption value are 589.27~669.15mg/g.
2. a kind of method for preparing charcoal using excess sludge and hazelnut shell copyrolysis according to claim 1, special Sign is that the concentration of liquor zinci chloridi in the step (3) is 2~5mol/L.
3. a kind of method for preparing charcoal using excess sludge and hazelnut shell copyrolysis according to claim 1, special Sign is that the temperature dried in the step (1), (3) and (5) is 100~110 DEG C, and the time is 22~26h.
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