CN108975305A - A method of carbon-based material is prepared using dewatered sludge - Google Patents
A method of carbon-based material is prepared using dewatered sludge Download PDFInfo
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- CN108975305A CN108975305A CN201810945559.XA CN201810945559A CN108975305A CN 108975305 A CN108975305 A CN 108975305A CN 201810945559 A CN201810945559 A CN 201810945559A CN 108975305 A CN108975305 A CN 108975305A
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- Prior art keywords
- carbon
- sludge
- based material
- carbonization treatment
- dewatered sludge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
Abstract
The invention belongs to wastewater treatments and recycling sludge to utilize technical field, disclose a kind of method for preparing carbon-based material using dewatered sludge, specific steps are as follows: (1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, Microwave-assisted firing carries out hydro-thermal reaction, obtains mixed liquor A'；(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, drying obtain mixed material A of the water content less than 10%；(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；(4) mixed material B is baked through low temperature；(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment；Then secondary carbonization treatment is carried out, carbon-based material is obtained.The application can be realized sludge and convert to the orientation of sludge carbon material, improve sludge carbon yield；Improve the content of the available phosphorus and available nitrogen in sludge carbon；Reduce the content of beary metal in sludge carbon.
Description
Technical field
The invention belongs to wastewater treatments and recycling sludge to utilize technical field, in particular to a kind of to utilize dewatered sludge system
The method of standby carbon-based material.
Background technique
Sludge is a kind of by-product of generation during sewage treatment plant's Aerobic biological process.According to the tune of relevant departments
It looks into, year end 2010 of China, China's urban wastewater treatment firm sewage treatment capacity was increased by 1.24 billion cubic meters/day to year ends 2015
To 1.7 billion cubic meters/day, the section for thus estimating sludge yield (moisture content 80%) is provided by ten thousand tons/year of 2200-4500
To ten thousand tons/year of 3000-6200.The growth of sewage load will lead to the lasting rising of sludge yield.But China by
It is limited in by factors such as economy, technology and management levels, the sewage sludge harmlessness disposing rate of domestic various regions sewage treatment plant is only
It is only about 56%, is often just simply filled without harmless treatment, notably unordered stockpiling, the ratio of sewage sludge harmlessness disposing is inclined
Low, this is far apart for 85.22% situation with China's urban wastewater treatment rate 91.90%, county town wastewater treatment rate.Sludge produces
Raw environmental problem is increasingly severe, this disposes dealing carefully with for sludge increasingly by the concern of the public.
Treatment of Sludge and the purpose of disposition are mainly by following 4 aspects: (1) minimizing, i.e., before reduction sludge ultimate disposal
Volume, to reduce the expense of Treatment of Sludge and final disposal；(2) it stabilizes, i.e., sludge stabilizing is made by processing, it is final to locate
The further degradation for no longer generating sludge is postponed, to avoid generating secondary pollution；(3) innoxious, that is, reach the harmless of sludge
Change and hygienization, such as go removing heavy metals or sterilizing；(4) recycling reaches while handling sludge and turns bane into boon, integrates
Using, protection environment purpose.Therefore, seek cost-effective minimizing, stabilisation, innoxious and recycling Treatment of Sludge
It is of great significance using technology.
It is the organic matter and nothing that the zoogloea formed by multiple-microorganism is adsorbed with it because the composition of sludge is complex
The aggregate of machine object composition.Sludge is a kind of rich carbon waste simultaneously, can be used as the raw material for preparing carbon material, and carbonization technique
Simply, the preparation of sludge Carbon Materials and application gain great popularity, and have become the research hotspot that recycling sludge utilizes.
Summary of the invention
The object of the present invention is to provide a kind of methods for preparing carbon-based material using dewatered sludge.
To achieve the goals above, the technical solution that the application uses are as follows: a kind of to prepare carbon-based material using dewatered sludge
Method, specific steps are as follows:
(1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, closed, controls hydrothermal reactor internal pressure
Power is 1atm~2atm, and heating temperature is 100 DEG C~200 DEG C, and Microwave-assisted firing carries out hydro-thermal reaction 30min~50min, obtains
To mixed liquor A'；
(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, 40 DEG C~60 DEG C dryings are contained
Mixed material A of the water less than 10%；
(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；
(4) mixed material B is baked to obtain through low temperature and bakes solid product and baking gaseous product；
(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment under the protection of inert gas, is obtained pre-
Carbonized product；Then pre- carbonized product is subjected to secondary carbonization treatment again, obtains carbon-based material.
Further, it bakes gaseous product to obtain cold oil by condensation and do not coagulate combustion gas, cold oil is used for and step (2)
Obtained mixed material A mixing.
Further, control microwave power is 100w~700w in step (1).
Further, control microwave power is 300w~500w in step (1).
Further, the stoving temperature of step (4) is 200 DEG C~300 DEG C, and the residence time is 3h~5h.
Further, the pre- carbonization treatment temperature of step (5) is 350 DEG C~500 DEG C, and the residence time is 1.5h~2.5h；Two
Secondary carbonization treatment temperature is 500 DEG C~800 DEG C, and the residence time is 0.5h~2h；The inert gas is in nitrogen or argon gas
One kind；
Further, not solidifying combustion gas caused by the gaseous product condensation process generates high temperature cigarette by burner combustion
Gas, high-temperature flue gas is as low temperature baking, the heat source of pre- carbonization treatment and secondary carbonization treatment process.
Further, the carbon-based material is sludge carbon.
Compared with prior art, it is converted the beneficial effects of the present invention are: can be realized sludge to the orientation of sludge carbon material,
To improve sludge carbon yield；The content of available phosphorus and available nitrogen in the sludge carbon of generation increased compared in raw sewage；
Content of beary metal in the sludge carbon of generation in raw sewage compared with decreasing.
Detailed description of the invention
Fig. 1 is a kind of method flow diagram that carbon-based material is prepared using dewatered sludge of the present invention.
Specific embodiment
Technological means of the invention, creation characteristic, achieving the goal is easy to understand with effect in order to make, below in conjunction with
The embodiment of the present invention and attached drawing, are clearly and completely described technical solution of the present invention.
It illustrates, the experimental material and reagent in the present invention are technical field regular market purchase product.
Embodiment 1
A method of carbon-based material, specific steps are prepared using dewatered sludge are as follows:
(1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, closed, controls hydrothermal reactor internal pressure
Power is 1atm, and heating temperature is 100 DEG C, and control microwave power is 100w, and Microwave-assisted firing carries out hydro-thermal reaction 30min, obtains
To mixed liquor A'；
(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, 40 DEG C of dryings obtain water content
1.3% mixed material A；
(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；
It bakes gaseous product to obtain cold oil by condensation and do not coagulate combustion gas, cold oil is used to obtain with step (2) mixed
Close material A mixing.It bakes and banks up with earth not solidifying combustion gas caused by gaseous product condensation process and generates high-temperature flue gas by burner combustion, it is high
Warm flue gas is as low temperature baking, the heat source of pre- carbonization treatment and secondary carbonization treatment process.
(4) mixed material B is baked to obtain through low temperature and bakes solid product and baking gaseous product；Wherein stoving temperature is
200 DEG C, residence time 3h.
(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment under the protection of inert gas, is obtained pre-
Carbonized product；Then pre- carbonized product is subjected to secondary carbonization treatment again, obtains carbon-based material, i.e. sludge carbon；Wherein pre- carbonization
Treatment temperature is 350 DEG C, residence time 1.5h；Secondary carbonization treatment temperature is 500 DEG C, residence time 0.5h；Indifferent gas
Body is nitrogen；
The yield of sludge carbon is 77.23% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 52.18%, is improved about using the yield of present invention process sludge carbon
25%.
Available phosphorus, available nitrogen have increased separately 41.19%, 44.64% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 83.23%, 85.81%.
Embodiment 2
A method of carbon-based material, specific steps are prepared using dewatered sludge are as follows:
(1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, closed, controls hydrothermal reactor internal pressure
Power is 2atm, and heating temperature is 200 DEG C, and control microwave power is 700w, and Microwave-assisted firing carries out hydro-thermal reaction 50min, obtains
To mixed liquor A'；
(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, 60 DEG C of dryings obtain water content
3.2% mixed material A；
(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；
It bakes gaseous product to obtain cold oil by condensation and do not coagulate combustion gas, cold oil is used to obtain with step (2) mixed
Close material A mixing.It bakes and banks up with earth not solidifying combustion gas caused by gaseous product condensation process and generates high-temperature flue gas by burner combustion, it is high
Warm flue gas is as low temperature baking, the heat source of pre- carbonization treatment and secondary carbonization treatment process.
(4) mixed material B is baked to obtain through low temperature and bakes solid product and baking gaseous product；Wherein stoving temperature is
300 DEG C, residence time 5h.
(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment under the protection of inert gas, is obtained pre-
Carbonized product；Then pre- carbonized product is subjected to secondary carbonization treatment again, obtains carbon-based material, i.e. sludge carbon；Wherein pre- carbonization
Treatment temperature is 500 DEG C, residence time 2.5h；Secondary carbonization treatment temperature is 800 DEG C, residence time 2h；Inert gas
For argon gas；
The yield of sludge carbon is 72.79% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 51.62%, is improved about using the yield of present invention process sludge carbon
20%.
Available phosphorus, available nitrogen have increased separately 39.75%, 35.46% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 80.54%, 88.96%.
Embodiment 3
A method of carbon-based material, specific steps are prepared using dewatered sludge are as follows:
(1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, closed, controls hydrothermal reactor internal pressure
Power is 1.5atm, and heating temperature is 150 DEG C, and control microwave power is 400w, and Microwave-assisted firing carries out hydro-thermal reaction 50min,
Obtain mixed liquor A'；
(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, 50 DEG C of dryings obtain water content
5.1% mixed material A；
(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；
It bakes gaseous product to obtain cold oil by condensation and do not coagulate combustion gas, cold oil is used to obtain with step (2) mixed
Close material A mixing.It bakes and banks up with earth not solidifying combustion gas caused by gaseous product condensation process and generates high-temperature flue gas by burner combustion, it is high
Warm flue gas is as low temperature baking, the heat source of pre- carbonization treatment and secondary carbonization treatment process.
(4) mixed material B is baked to obtain through low temperature and bakes solid product and baking gaseous product；Wherein stoving temperature is
250 DEG C, residence time 4h.
(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment under the protection of inert gas, is obtained pre-
Carbonized product；Then pre- carbonized product is subjected to secondary carbonization treatment again, obtains carbon-based material, i.e. sludge carbon；Wherein pre- carbonization
Treatment temperature is 420 DEG C, residence time 2h；Secondary carbonization treatment temperature is 650 DEG C, residence time 1.5h；Inert gas
For argon gas；
The yield of sludge carbon is 78.92% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 53.49%, is improved about using the yield of present invention process sludge carbon
25%.
Available phosphorus, available nitrogen have increased separately 43.43%, 45.29% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 81.54%, 89.81%.
Embodiment 4
Different from embodiment 3 is only control microwave power, and the control microwave power of embodiment 4 is 300w.
The yield of sludge carbon is 76.79% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 51.89%, is improved about using the yield of present invention process sludge carbon
25%.
Available phosphorus, available nitrogen have increased separately 42.72%, 44.64% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 84.03%, 90.11%.
Embodiment 5
Different from embodiment 3 is only control microwave power, and the control microwave power of embodiment 5 is 500w.
The yield of sludge carbon is 79.03% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 53.88%, is improved about using the yield of present invention process sludge carbon
25%.
Available phosphorus, available nitrogen have increased separately 39.94%, 42.84% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 82.43%, 88.81%.
Embodiment 6
Different from embodiment 3 is only control microwave power, and the control microwave power of embodiment 6 is 600w.
The yield of sludge carbon is 76.23% under process conditions used in the present embodiment, straight at 800 DEG C of common process of comparison
The dry sludge of carbonization is connect, the yield of obtained sludge carbon is about 50.18%, is improved about using the yield of present invention process sludge carbon
25%.
Available phosphorus, available nitrogen have increased separately 40.09%, 41.34% compared with raw sewage in the sludge carbon that the present embodiment obtains,
Also contain a large amount of carbons and nutritional ingredient.The content in the leaching liquor of Cd, Cu is measured to its heavy metal to distinguish compared with raw sewage
Reduce 81.63%, 88.21%.
In conclusion the sludge that can be realized of the application is converted to the orientation of sludge carbon material, sludge carbon yield is more traditional
Technique improves 25%；The content of available phosphorus and available nitrogen in the sludge carbon of generation is compared with increasing by 40% in raw sewage；It generates
Content of beary metal in sludge carbon is compared with reducing by 80% in raw sewage.
Disclosed above is only presently preferred embodiments of the present invention, and still, the embodiment of the present invention is not limited to this, Ren Heben
What the technical staff in field can think variation should all fall into protection scope of the present invention.
Claims (8)
1. a kind of method for preparing carbon-based material using dewatered sludge, which is characterized in that specific steps are as follows:
(1) hydro-thermal process: sewage plant dewatered sludge is sent into hydrothermal reactor, closed, is controlled pressure in hydrothermal reactor and is
1atm~2atm, heating temperature are 100 DEG C~200 DEG C, and Microwave-assisted firing carries out hydro-thermal reaction 30min~50min, is mixed
Close feed liquid A'；
(2) obtained mixed liquor A' is separated by solid-liquid separation, solid product washing, 40 DEG C~60 DEG C dryings obtain water content
Mixed material A less than 10%；
(3) mix: mixed material A is uniformly mixed with cold oil, obtains mixed material B；
(4) mixed material B is baked to obtain through low temperature and bakes solid product and baking gaseous product；
(5) carbonization treatment: solid product will be baked first and carries out pre- carbonization treatment under the protection of inert gas, obtains pre- carbonization
Product；Then pre- carbonized product is subjected to secondary carbonization treatment again, obtains carbon-based material.
2. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that bake gaseous product
Cold oil is obtained by condensation and does not coagulate combustion gas, and the mixed material A that cold oil is used to obtain with step (2) is mixed.
3. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that control in step (1)
Microwave power processed is 100w~700w.
4. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that control in step (1)
Microwave power processed is 300w~500w.
5. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that the baking of step (4)
Roasting temperature is 200 DEG C~300 DEG C, and the residence time is 3h~5h.
6. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that step (5) pre- carbon
Changing treatment temperature is 350 DEG C~500 DEG C, and the residence time is 1.5h~2.5h；Secondary carbonization treatment temperature is 500 DEG C~800 DEG C,
Residence time is 0.5h~2h；The inert gas is one of nitrogen or argon gas.
7. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that the baking gas
Not solidifying combustion gas caused by product condensation process generates high-temperature flue gas by burner combustion, high-temperature flue gas as low temperature baking,
The heat source of pre- carbonization treatment and secondary carbonization treatment process.
8. the method for preparing carbon-based material using dewatered sludge as described in claim 1, which is characterized in that the carbon-based material
For sludge carbon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113307462A (en) * | 2021-06-11 | 2021-08-27 | 安徽尘缘节能环保科技有限公司 | Harmless treatment and resource utilization method of sludge |
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| DE102008004732A1 (en) * | 2008-01-16 | 2009-07-23 | Lucia Viviane Sanders | Hydrothermal carbonization of biomass |
| CN104150743A (en) * | 2014-07-22 | 2014-11-19 | 广州中国科学院先进技术研究所 | Method for preparing sludge carbon by virtue of microwave-assisted hydrothermal carbonization |
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| CN105417918A (en) * | 2015-12-08 | 2016-03-23 | 深圳大学 | Technical method for treating civil sludge through microwave pyrolysis |
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Application publication date: 20181211 |