CN106966562A - A kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value - Google Patents
A kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value Download PDFInfo
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- CN106966562A CN106966562A CN201710321780.3A CN201710321780A CN106966562A CN 106966562 A CN106966562 A CN 106966562A CN 201710321780 A CN201710321780 A CN 201710321780A CN 106966562 A CN106966562 A CN 106966562A
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- Prior art keywords
- reactor
- sludge
- oil
- heating value
- high heating
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010802 sludge Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000010438 heat treatment Methods 0.000 title claims abstract description 27
- 239000012075 bio-oil Substances 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 title claims abstract description 16
- 239000012530 fluid Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010792 warming Methods 0.000 claims abstract description 13
- 239000003125 aqueous solvent Substances 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 3
- 238000007710 freezing Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000126 substance Substances 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 description 14
- 239000012046 mixed solvent Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 238000004064 recycling Methods 0.000 description 3
- 239000011449 brick Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention provides a kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value, city organic sludge is first dried into 8 ~ 20h at 100 ~ 120 DEG C；Then the city organic sludge is freezed and stored at 30 ~ 10 DEG C；The sludge of the freezing is warming up to 0 ~ 10 DEG C again, is fitted into reactor, and the addition alcohol aqueous solvent into reactor, and being passed through nitrogen makes reactor be pressurized to 1 ~ 10MPa；Reactor is stirred under 100 ~ 1000rpm speed again, and is heated to 250 ~ 500 DEG C；Reactor is finally stopped to 10 ~ 50 min at such a temperature, the liquid bio-oil of high heating value is obtained.Present invention process flow is simple, and process cycle is short, recycles valuable organic matter yield height in sludge, can preferably solve conventional process mode and pollute the problems such as environment, valuable substance yield are few, be adapted to industrial application.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of method for sludge treatment, specifically one kind utilizes supercritical fluid
The method for handling the liquid bio-oil of municipal sludge production high heating value.
Background technology
With China's economy and the fast development of urbanization, the discharge capacity of China's municipal sewage is growing day by day.It is to environment
The negative effect caused also gradually causes global concern.
City organic sludge is as the secondary product in sewage treatment plant's sewage disposal process, with adding for Development of China's Urbanization
Necessarily increase rapidly soon.At present, the developed country such as America and Europe municipal sludge process field development relative maturity, in state
It is interior, build the data analysis in portion according to living, the annual dewatered sludge amount of China alreadys exceed 32,000,000 tons, and at present still with annual 5% ~
10% speed increases.City organic sludge water content is high, it is smelly easily to degenerate, containing plurality of heavy metal and some difficult degradations
Poisonous and harmful substance so as to causing its difficult.How rationally, effectively processing sludge has turned into one and very urgent asked
Topic.
Containing organic compound enrich and valuable and nutrient in municipal sludge, China handles the biography of municipal sludge
System method mainly has landfill, burning and recycling.It is tight using the method processing municipal sludge environmental pollution of landfill
Moisture meeting osmosis pollution underground water in weight, sludge, and valuable material is not reclaimed completely in sludge；Utilize the side of burning
Method processing municipal sludge investment is big, and equipment running cost is high, and can produce the extremely toxic substances such as bioxin during burning；Utilize sludge
Recycling handles sludge such as making brick from sludge, and brickmaking energy consumption is higher and brick quality is relatively low caused by water content is higher in sludge,
Toxic and harmful gas can be produced in sintering procedure；The agricultural quality requirement to sludge is higher after sludge composting, and is needed before compost
High-temperature process is carried out to sludge, processing cost is higher.Processing municipal sludge is once dealt with improperly in aforementioned manners, it is most likely that right
Environment causes secondary pollution.Therefore, the recycling and recovery energy of sludge will be the following important development of domestic sludge industry
Direction.
The content of the invention
It is dirty using treatment with supercritical fluid city the invention provides one kind for above-mentioned technical problem of the prior art
The method of the liquid bio-oil of mud production high heating value, described this utilization treatment with supercritical fluid municipal sludge production high heating value
The method of liquid bio-oil to solve to handle the method for municipal sludge in the prior art and easily cause the technology of secondary pollution and ask
Topic.
The invention provides a kind of side of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value
Method, is comprised the steps of：
1) the step of being pre-processed city organic sludge, described pretreatment refers to city organic sludge 100 ~ 120
8 ~ 20h is dried at DEG C；
2) the city organic sludge is being freezed and stored at -30 ~ -10 DEG C；
3) sludge of the freezing is warming up to 0 ~ 10 DEG C, be fitted into reactor, and the addition alcohol aqueous solvent into reactor, and lead to
Entering nitrogen makes reactor be pressurized to 1 ~ 10MPa；
4) reactor is stirred under 100 ~ 1000rpm speed, and heats 250 ~ 500 DEG C；
5) reactor is stopped to 10 ~ 50 min at such a temperature, the liquid bio-oil of high heating value is obtained.
Further, in described alcohol aqueous solvent, the volume ratio of alcohol and water is 0 ~ 10:10 ~ 0, described alcohol is ethanol
Or methanol.
Further, step 5）In temperature be 300 ~ 500 DEG C.
Further, step 5）Middle stop 30min.
Further, the air for being purged with nitrogen and being remained to remove in reactor is adopted.The purpose for being passed through nitrogen is to allow sludge
The bio oil of high heating value is pyrolyzed under conditions of anaerobic and supercritical fluid.
Further, step 3）In, being passed through nitrogen makes reactor be pressurized to 1MPa.
The present invention utilizes the organic sludge of municipal sewage plant, it is not necessary to catalyst is added, at supercritical fluid
The method of reason produces the liquid bio-oil of high heating value.
The present invention is compared with prior art, and its technological progress is significant.Present invention process flow is simple, process cycle
It is short, recycle in sludge that valuable organic matter yield is high, can preferably solve conventional process mode pollute environment, it is valuable
The problems such as material yield is few, is adapted to industrial application.
Embodiment
The embodiment that the present invention is provided is elaborated below.
Embodiment 1：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that ethanol and water are added into reactor is 3:7 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 242%.
Embodiment 2：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 10:0 mixed solvent, be purged with nitrogen three times with
The air remained in reactor is removed, and being passed through nitrogen makes reactor be pressurized to 1MPa, with 500rmp speed stirring and with 15
DEG C/min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 213%.
Embodiment 3：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 7:3 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 221%.
Embodiment 4：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 5:5 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 231%.
Embodiment 5：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 0:10 mixed solvent, be purged with nitrogen three times with
The air remained in reactor is removed, and being passed through nitrogen makes reactor be pressurized to 1MPa, with 500rmp speed stirring and with 15
DEG C/min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 235%.
Embodiment 6：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 10:0 mixed solvent, be purged with nitrogen three times with
The air remained in reactor is removed, and being passed through nitrogen makes reactor be pressurized to 1MPa, with 500rmp speed stirring and with 15
DEG C/min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 203%.
Embodiment 7：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that ethanol and water are added into reactor is 7:3 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 223%.
Embodiment 8：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that ethanol and water are added into reactor is 5:5 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 221%.
Embodiment 9：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that ethanol and water are added into reactor is 0:10 mixed solvent, be purged with nitrogen three times with
The air remained in reactor is removed, and being passed through nitrogen makes reactor be pressurized to 1MPa, with 500rmp speed stirring and with 15
DEG C/min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 235%.
Embodiment 10：
Sample is dried at 105 DEG C and freezes and is stored in -20 DEG C of environment after 12h until using；Sludge is warming up to 4 DEG C,
It is put into reactor, the volume ratio that methanol and water are added into reactor is 3:7 mixed solvent, is purged with nitrogen three times to go
Except the air remained in reactor, and being passed through nitrogen makes reactor be pressurized to 1MPa, with the stirring of 500rmp speed and with 15 DEG C/
Min speed heating response device is heated to 400 DEG C of stop 30min.Compared with raw sewage, calorific value increase by 237%.
Claims (5)
1. a kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value, it is characterised in that bag
Containing following steps：
1）The step of city organic sludge is pre-processed, described pretreatment refers to city organic sludge 100 ~ 120
8 ~ 20h is dried at DEG C；
2）The city organic sludge is being freezed and stored at -30 ~ -10 DEG C；
3）The sludge of the freezing is warming up to 0 ~ 10 DEG C, is fitted into reactor, and the addition alcohol aqueous solvent into reactor, and lead to
Entering nitrogen makes reactor be pressurized to 1 ~ 10MPa；
4）Reactor is stirred under 100 ~ 1000rpm speed, and is heated to 250 ~ 500 DEG C；
5）Reactor is stopped to 10 ~ 50 min at such a temperature, the liquid bio-oil of high heating value is obtained.
2. a kind of liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value as claimed in claim 1
Method, it is characterised in that：In described alcohol aqueous solvent, the volume ratio of alcohol and water is 0 ~ 10:10 ~ 0, described alcohol for ethanol or
Person's methanol.
3. a kind of liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value as claimed in claim 1
Method, it is characterised in that：Step 5）In temperature be 300 ~ 500 DEG C.
4. a kind of liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value as claimed in claim 1
Method, it is characterised in that：Step 5）Middle stop 30min.
5. a kind of liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value as claimed in claim 1
Method, it is characterised in that：Step 3）In, being passed through nitrogen makes reactor be pressurized to 1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710321780.3A CN106966562A (en) | 2017-05-09 | 2017-05-09 | A kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710321780.3A CN106966562A (en) | 2017-05-09 | 2017-05-09 | A kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106966562A true CN106966562A (en) | 2017-07-21 |
Family
ID=59330708
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710321780.3A Pending CN106966562A (en) | 2017-05-09 | 2017-05-09 | A kind of method of the liquid bio-oil of utilization treatment with supercritical fluid municipal sludge production high heating value |
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| Country | Link |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746723A (en) * | 2017-11-06 | 2018-03-02 | 沈阳航空航天大学 | A kind of method that sludge liquefaction prepares bio-fuel |
| CN107880924A (en) * | 2017-11-09 | 2018-04-06 | 沈阳航空航天大学 | A kind of liquefied in the mixed solvent prepares the process of bio oil |
| CN108659876A (en) * | 2018-05-18 | 2018-10-16 | 沈阳航空航天大学 | The method for preparing bio oil is combined in pretreatment of raw material with hydrothermal liquefaction |
| CN110467327A (en) * | 2019-07-11 | 2019-11-19 | 佛山科学技术学院 | A kind of method of ethyl alcohol pyrolysis sewage treatment plant excess sludge liquefaction oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911691A (en) * | 2012-11-05 | 2013-02-06 | 天津大学 | Method for preparing bio-oil through supercritical pyrolysis of civil sludge |
| CN106277676A (en) * | 2016-08-31 | 2017-01-04 | 王焕升 | A kind of for disposing the chemical industry danger device of waste sludge and technique |
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2017
- 2017-05-09 CN CN201710321780.3A patent/CN106966562A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911691A (en) * | 2012-11-05 | 2013-02-06 | 天津大学 | Method for preparing bio-oil through supercritical pyrolysis of civil sludge |
| CN106277676A (en) * | 2016-08-31 | 2017-01-04 | 王焕升 | A kind of for disposing the chemical industry danger device of waste sludge and technique |
Non-Patent Citations (1)
| Title |
|---|
| 刘京等: "市政污泥在超临界甲醇条件下酯化制油研究", 《中国给水排水》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746723A (en) * | 2017-11-06 | 2018-03-02 | 沈阳航空航天大学 | A kind of method that sludge liquefaction prepares bio-fuel |
| CN107746723B (en) * | 2017-11-06 | 2020-04-10 | 沈阳航空航天大学 | Method for preparing biofuel by liquefying sludge |
| CN107880924A (en) * | 2017-11-09 | 2018-04-06 | 沈阳航空航天大学 | A kind of liquefied in the mixed solvent prepares the process of bio oil |
| CN108659876A (en) * | 2018-05-18 | 2018-10-16 | 沈阳航空航天大学 | The method for preparing bio oil is combined in pretreatment of raw material with hydrothermal liquefaction |
| CN110467327A (en) * | 2019-07-11 | 2019-11-19 | 佛山科学技术学院 | A kind of method of ethyl alcohol pyrolysis sewage treatment plant excess sludge liquefaction oil |
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Application publication date: 20170721 |
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