CN105295981B - A kind of method for lifting pyrolyzing sludge oil quality - Google Patents
A kind of method for lifting pyrolyzing sludge oil quality Download PDFInfo
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- CN105295981B CN105295981B CN201510662755.2A CN201510662755A CN105295981B CN 105295981 B CN105295981 B CN 105295981B CN 201510662755 A CN201510662755 A CN 201510662755A CN 105295981 B CN105295981 B CN 105295981B
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- 239000010802 sludge Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000197 pyrolysis Methods 0.000 claims abstract description 21
- 238000010792 warming Methods 0.000 claims abstract description 18
- 239000002028 Biomass Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 11
- 235000007164 Oryza sativa Nutrition 0.000 claims description 8
- 235000009566 rice Nutrition 0.000 claims description 8
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 5
- 244000105624 Arachis hypogaea Species 0.000 claims description 5
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 5
- 235000018262 Arachis monticola Nutrition 0.000 claims description 5
- 235000020232 peanut Nutrition 0.000 claims description 5
- 241000609240 Ambelania acida Species 0.000 claims description 4
- 235000014676 Phragmites communis Nutrition 0.000 claims description 4
- 239000010905 bagasse Substances 0.000 claims description 4
- 239000010903 husk Substances 0.000 claims description 4
- 239000010841 municipal wastewater Substances 0.000 claims description 4
- 239000010902 straw Substances 0.000 claims description 4
- 240000007594 Oryza sativa Species 0.000 claims 2
- 240000003826 Eichhornia crassipes Species 0.000 claims 1
- 230000011218 segmentation Effects 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 230000007812 deficiency Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 26
- 241000209094 Oryza Species 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 241000169203 Eichhornia Species 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- 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
Landscapes
- Processing Of Solid Wastes (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention provides a kind of method for lifting pyrolyzing sludge oil quality, sludge and abandoned biomass and catalyst are pressed 1 by it:(1.0~1.5):(0.01~0.05) weight is than mixing; it is placed in the fixed bed reactors under nitrogen protection; pyrolysis is segmented by certain heating schedule; progressively it is warming up to 550 DEG C; the gas of generation is condensed in condensing unit; gained is pyrolyzed oily yield and quality is higher than pure sludge pyrolytic oil under the same terms, is respectively：Oil productivity (moisture-free basis) 35%~45%, 30~35MJ/kg of Lower heat value, 15~18mm of viscosity2/g.The present invention utilizes abandoned biomass and sludge copyrolysis, the advantage of abandoned biomass and each self-pyrolysis of sludge is made full use of, is made up for each other's deficiencies and learn from each other, pyrolyzing sludge oil quality is lifted, the problem of environmental pollution of two kinds of discarded objects is solved, cleaning, the high-efficiency resource recycling of two kinds of discarded objects is realized.
Description
Technical field
Abandoned biomass is utilized the present invention relates to a kind of method of waste remediation and recycling, more particularly to one kind
The method that pyrolyzing sludge oil quality is lifted with sludge copyrolysis.
Background technology
Environmental pollution and energy crisis have become the two large problems of today's society presence, receive the extensive of various circles of society
Concern.How while energy demand is met, and earth environment for the survival of mankind can be protected to turn into the heat of scientific research instantly
One of point.And the sludge (abbreviation sludge) of municipal wastewater treating stations, as a kind of complicated component, discharge capacity is huge, and environmental toxicity is strong
Sewage purification accessory substance, it is carried out minimizing, stabilisation, recycling, innoxious processing receive it is both domestic and external common
Concern.Compared with traditional burning, filling, doing the processing methods such as building filler, compost, pyrolytic technique processing sludge has substantially
Advantage.Pyrolyzing sludge can not only produce liquid oil and fuel gas, while contained heavy metal is passivated, and bioxin is generated
Amount is significantly reduced, and greatly reduces the secondary pollution of sludge handling process.There are many similar property to oil in sludge pyrolytic oil
Matter, can be thus interested to researchers in recent years as fuel or other chemicals.Because of the different pyrolysis oils of the mode of production
Change of properties is very big, and the features such as low yield, acid number are larger, water content is high, calorific value is low, viscosity is difficult to greatly conveying affects sludge hot
The application of oil is solved, the development of pyrolyzing sludge technology is also limit.
The content of the invention
It is an object of the invention to overcome obtained by the existing pyrolytic technique of sludge, pyrolysis oil viscosity is higher, acid number is larger, yield
Low the problem of, there is provided a kind of method for lifting pyrolyzing sludge oil quality.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of method for lifting pyrolyzing sludge oil quality, 1 is pressed by sludge, abandoned biomass and catalyst:1.0~1.5:
0.01~0.05 weight is placed in the fixed bed reactors under nitrogen protection than mixing, is segmented and is pyrolyzed by certain heating schedule,
550 DEG C of final temperature is progressively warming up to, the gas of generation is condensed in condensing unit, that is, obtains higher than pure pyrolyzing sludge oil quality
Pyrolysis oil.
The heating schedule is：First with 20 DEG C/min programming rate from room temperature to 275 DEG C, constant temperature 10 minutes；
Be warming up to 450 DEG C from 275 DEG C again with 20 DEG C/min programming rate, constant temperature 10 minutes, then with 20 DEG C/min programming rate from
450 DEG C are warming up to 550 DEG C of final temperature, constant temperature 20 minutes.
The sludge be municipal wastewater treating stations filter sludge, 10~15wt% of its moisture content, granular size be less than
1mm；The abandoned biomass is the one or more in peanut shell, water hyacinth, rice husk, rice straw, reed Leaves and bagasse, particle
Size is less than 1mm；The catalyst is oyster shell ash, and granular size is less than 0.1mm.
After adopting the above technical scheme, the inventive method is blended and a small amount of using abandoned biomass with sludge by proper proportion
Catalyst copyrolysis, utilizes the distinctive composition structural improvement pyrolyzing sludge process of biomass.The characteristics of biomass is that organic matter contains
Amount is high, and the calorific value of thermal decomposition product is high, but solid product density is low, easily wafts, be difficult to store and transport, and the aqueous high, calorific value of sludge is low, liquid
Body product assay is low, solid product density big, while viscosity is difficult to convey greatly.Both materials are mixed in suitable ratio,
It can then learn from other's strong points to offset one's weaknesses.The distinctive fibre structure of biomass can increase the porosity of pyrolyzing sludge process, reduce pyrolyzing sludge mistake
The reaction resistance of journey；In biomass pyrolysis process, due to the quick generation of cracking process chain reaction process, a large amount of hydrogen are generated
Free radical, methyl free radicals etc. so that pyrolyzing sludge has more chain reaction to trigger group in high temperature environments, and in hydrogen
In the presence of free radical the reproducibility in inert atmosphere is strengthened, be more beneficial for alkane and ester type compound life
Into so as to lift pyrolysis oil quality；Catalyst is added during copyrolysis, point of thermal decomposition product can be optionally controlled
Cloth, increases the yield of some specific target products, suppresses some compositions, and the especially generation of acids improves pyrolysis oil
Quality.
It is an advantage of the current invention that while lifting pyrolyzing sludge oil quality, realizing innoxious, the money of two kinds of discarded objects
Sourceization is utilized, and has reached the purpose of environmental protection, changing rejected material to useful resource, sustainable development, has had important meaning to the economic construction of China
Justice.
Effect of the invention is that, the pyrolysis oil oil productivity (moisture-free basis) 35% obtained using above-mentioned technical proposal~
45%th, 30~35MJ/kg of Lower heat value, 15~18mm of viscosity2/g.When GC-MS analysis pyrolysis oil main components understand copyrolysis
The species of the higher component of content is significantly reduced, only four major classes, illustrates that copyrolysis process is conducive to the composition of pyrolysis oil more
Unification, facilitates follow-up deep processing and utilization.Contrast variety classes compound relative amount is it can be found that biomass and sludge are total to
Pyrolysis gained pyrolysis oil is individually pyrolyzed the pyrolysis oil of gained compared to sludge, and the content of esters is obviously improved, thus significantly
Pyrolysis oil acid number and viscosity are reduced, is that the later use of pyrolysis oil is provided convenience.
Embodiment
A kind of method for lifting pyrolyzing sludge oil quality of the present invention, is achieved by the following scheme：
Sludge, abandoned biomass and catalyst are pressed 1:(1.0~1.5):The weight of (0.01~0.05) is placed in than mixing
In fixed bed reactors under nitrogen protection, it is pyrolyzed by certain heating schedule temperature-gradient method, is finally warming up to 550 DEG C, generation
Gas condensed in condensing unit, that is, obtain the pyrolysis oil higher than pure pyrolyzing sludge oil quality.
Wherein：
Fixed bed reactors used are 400 × 600mm of φ programmable temperature control fixed bed reactors, described heating journey
Sequence is specific as follows：First with 20 DEG C/min programming rate from room temperature to 275 DEG C, constant temperature 10 minutes；Again with 20 DEG C/min
Programming rate be warming up to 450 DEG C from 275 DEG C, constant temperature 10 minutes, then end is warming up to from 450 DEG C with 20 DEG C/min programming rate
550 DEG C of temperature, constant temperature 20 minutes.
Sludge use municipal wastewater treating stations filter sludge, 10~15wt% of its moisture content, granular size be less than
1mm。
Abandoned biomass uses the one or more in peanut shell, water hyacinth, rice husk, rice straw, reed Leaves and bagasse,
Grain size is less than 1mm.
Catalyst is using oyster shell ash, and granular size is less than 0.1mm.
Embodiment 1：
Sludge, peanut shell and oyster shell ash press 1:1.0:0.01 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The pyrolysis oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
36.23%th, calorific value is 33.08MJ/kg, viscosity 18.06mm2/g；
Embodiment 2：
Sludge, water hyacinth and oyster shell ash press 1:1.2:0.03 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The biological oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
39.63%th, calorific value 33.58MJ/kg, viscosity 17.34mm2/g；
Embodiment 3：
Sludge, bagasse and oyster shell ash press 1:1.0:0.01 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The biological oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
40.38%th, calorific value 34.12MJ/kg, viscosity 16.17mm2/g；
Embodiment 4：
Sludge, reed Leaves and oyster shell ash press 1:1.0:0.01 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The pyrolysis oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
35.13%th, calorific value is 30.08MJ/kg, viscosity 17.03mm2/g；
Embodiment 5：
Sludge, rice straw and oyster shell ash press 1:1.0:0.01 weight is laid in quartzy Noah's ark, put than mixing, common 60g
In φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The biological oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
39.82%th, calorific value 36.49MJ/kg, viscosity 16.85mm2/g；
Embodiment 6：
Sludge, rice husk and oyster shell ash press 1:1:0.03 weight is laid in quartzy Noah's ark, is placed in than mixing, common 60g
In φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, is segmented and is pyrolyzed by foregoing heating schedule,
Progressively it is warming up to 550 DEG C.Biological oily yield (moisture-free basis) 41.63% that the gas of generation is obtained after being condensed in condensing unit,
Calorific value 38.78MJ/kg, viscosity 15.48mm2/g；
Embodiment 7：
Sludge, water hyacinth and oyster shell ash press 1:1.5：0.03 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The biological oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
43.63%th, calorific value 34.78MJ/kg, viscosity 16.88mm2/g；
Embodiment 8：
Sludge, peanut shell and oyster shell ash press 1:1.5:0.05 weight is laid in quartzy Noah's ark than mixing, common 60g,
It is placed in φ 400 × 600mm fixed bed reactors, nitrogen protection air-flow amount is 250mL/min, and heat is segmented by foregoing heating schedule
Solution, is progressively warming up to 550 DEG C.The biological oily yield (moisture-free basis) that the gas of generation is obtained after being condensed in condensing unit
44.67%th, calorific value 35.02MJ/kg, viscosity 15.29mm2/g。
Claims (2)
1. a kind of method for lifting pyrolyzing sludge oil quality, it is characterised in that：Sludge, abandoned biomass and catalyst are pressed 1:
1.0~1.5:0.01~0.05 weight is placed in the fixed bed reactors under nitrogen protection, by certain heating schedule than mixing
Segmentation pyrolysis, is progressively warming up to 550 DEG C of final temperature, the gas of generation is condensed in condensing unit, that is, obtained than pure sludge pyrolytic oil
The higher pyrolysis oil of quality；
The sludge is the filter sludge of municipal wastewater treating stations, and 10~15wt% of its moisture content, granular size is less than 1mm；
The abandoned biomass is the one or more in peanut shell, water hyacinth, rice husk, rice straw, reed Leaves and bagasse, granular size
For less than 1mm；The catalyst is oyster shell ash, and granular size is less than 0.1mm.
2. a kind of method for lifting pyrolyzing sludge oil quality according to claim 1, it is characterised in that：The heating schedule
For：First with 20 DEG C/min programming rate from room temperature to 275 DEG C, constant temperature 10 minutes；Again with 20 DEG C/min heating speed
Degree is warming up to 450 DEG C from 275 DEG C, constant temperature 10 minutes, then 550 DEG C of final temperature is warming up to from 450 DEG C with 20 DEG C/min programming rate,
Constant temperature 20 minutes.
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| CN201510662755.2A CN105295981B (en) | 2015-10-14 | 2015-10-14 | A kind of method for lifting pyrolyzing sludge oil quality |
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| CN107663002A (en) * | 2016-07-28 | 2018-02-06 | 华云新能源科技（深圳）有限公司 | A kind of sludge method for cracking treatment and equipment |
| CN106433713A (en) * | 2016-11-01 | 2017-02-22 | 新疆大学 | Sludge pyrolysis method adopting biomass adding |
| CN106977068A (en) * | 2017-04-14 | 2017-07-25 | 中国科学院广州能源研究所 | A kind of method for improving sludge carbon yield |
| CN108587669B (en) * | 2018-05-18 | 2019-11-26 | 武汉理工大学 | A kind of shale gas oil-based drill cuttings resource utilization method |
| CN115780480B (en) * | 2022-09-26 | 2024-05-28 | 山东大学 | Pyrolysis method of oil-containing dead catalyst |
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| CN101643687A (en) * | 2009-08-24 | 2010-02-10 | 中国矿业大学 | Oil producing technology for co-pyrolysis of municipal sewage sludge and agricultural waste |
| CN102936087B (en) * | 2012-11-06 | 2014-06-04 | 大连海事大学 | Method for preparing pyrolysis oil and synthesis gases by pyrolysis of sludge |
| CN103396820B (en) * | 2013-07-04 | 2015-05-20 | 北京林业大学 | Method for preparing bio-oil through biomass pyrolysis |
| WO2015089442A1 (en) * | 2013-12-14 | 2015-06-18 | Anellotech, Inc. | Catalysts and processes for producing p-xylene from biomass |
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