CN105087036A - Method for quickly pyrolyzing sludge to prepare bio-oil and soil improver by microwave assisted catalysis - Google Patents
Method for quickly pyrolyzing sludge to prepare bio-oil and soil improver by microwave assisted catalysis Download PDFInfo
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- CN105087036A CN105087036A CN201510440143.9A CN201510440143A CN105087036A CN 105087036 A CN105087036 A CN 105087036A CN 201510440143 A CN201510440143 A CN 201510440143A CN 105087036 A CN105087036 A CN 105087036A
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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
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Abstract
The invention relates to a method for quickly pyrolyzing sludge to prepare bio-oil and a soil improver by microwave assisted catalysis. The method comprises the following steps: (1) weighing silicon carbide spherical particles and a HZSM-5 spherical catalyst in a mass ratio of 1: 1 to 1: 2, and uniformly mixing and adding the mixture into a quartz reaction kettle; (2) putting the quartz reaction kettle in a microwave splitting instrument, heating the quartz reaction kettle to 450-600 DEG C, stirring the mixture at a rate of 60-100 r/minute, gradually adding dried sludge powder into the quartz reaction kettle and condensing the generated steam to obtain a brown liquid product bio-oil, and collecting solid residues as the soil improver. The method provided by the invention is simple in process and quick to split, and the obtained split fuel is high in hydrocarbon content which can reach over 55%. The obtained split fuel comprises important chemical raw materials such as naphthalene, p-xylene, 1,3,5-trimethylbenzene, 1-methylnaphthalene, indene and the like. The obtained solid residues are very high in content of P, Ca, K and Mg and can be used as the soil improver to improve the soil fertility.
Description
Technical field
The invention belongs to biomass energy transformation technology field.
Background technology
Along with to the concern of environment protection and the expansion in city, along with how successfully managing growing sewage, mud becomes a vital problem.Containing features such as a large amount of heavy metals (as As, Cd, Cr, Hg, Pb, Cu, Zn, Ni), virus, pathogenic bacterium, worm's ovum and difficult degradation toxic organic compounds in mud, if incorrect process, be easy to cause serious secondary pollution to environment.The handling problems national governments of mud are all explicitly called for and follows minimizing, stabilization, resource utilization, innoxious principle.
Utilize pyrolytic technique sewage sludge to be a kind of excellent technique of resourcebility, be day by day subject to extensive concern, there is wide development space.But due to the complicacy of sludge components, in pyrolysis oil oxygenatedchemicals and nitrogenous compound more, and complicated component, be difficult to utilize, the quality rationally improving the gas, liquid, solid three-phase product of pyrolyzing sludge economically becomes urgent problem.
One of key factor hindering quality of bio-oil and productive rate to improve in conventional pyrolytic technique is that temperature rise rate is slow, causes reactant to stop low-temperature condition for a long time.Microwave absorbing material add the intensification behavior changing raw material, solve the pyrolysis of traditional microwave matter and pursue be rapidly heated " focus " negative effect caused, the efficient transmission that microwave energy can be strengthened and absorption, the bottleneck that heat conduction efficiency in breakthrough heat-processed is low, significantly reduces thermosteresis.Microwave heating is compared traditional heating and have plurality of advantages in biomass pyrolytic, but in the research process of microwave-assisted cracking mud, do not find good catalysts selective all the time, improve the unicity of cracking bio oil composition, and reduce the content containing oxygen nitrogenous compound in cracking bio oil.
Summary of the invention
A kind of micro ware auxiliary catalysis fast pyrogenation of object of the present invention mud prepares the method for bio oil and soil improvement agent.
The present invention is achieved by the following technical solutions.
A kind of micro ware auxiliary catalysis fast pyrogenation mud of the present invention prepares the method for bio oil and soil improvement agent, comprises the following steps.
(1) by silicon carbide spheroidal particle: the mass ratio of HZSM-5 spherical catalyst=1:1 ~ 1:2, take silicon carbide spheroidal particle, HZSM-5 spherical catalyst, mix and add in quartz reaction still.
(2) quartz reaction still is placed in microwave cracking instrument, is heated to 450 ~ 600 DEG C, stirring velocity is 60-100r/min, add sludge-drying powder gradually, by the vapor condensation produced, obtain brown liquid product bio oil, and collect solid residue and make soil improvement agent.
Silicon carbide spherical particle diameters of the present invention is 5mm-20mm.
HZSM-5 spherical catalyst particles diameter of the present invention is 5mm-20mm, Si/C=20-40, specific surface area 380-450m
2/ g.
Sludge-drying powder of the present invention comprises the mud of municipal sewage, by dry 72h at 80 ± 1 DEG C of temperature, crosses 2mm sieve after pulverizing.
The present invention has the following advantages.
1, technique is simple, cracking is quick, gained cracking hydrocarbon oil aromatic hydrocarbon content is high, can reach more than 55%, comprising naphthalene, p-Xylol, 1,3, the important industrial chemicals such as 5-trimethylbenzene, 1-methylnaphthalene and indenes, P in gained solid residue, Ca, the content of K and Mg is very high, can improve fertile soil degree as soil improvement agent.
2, HZSM-5 catalyzer has satisfactory stability, can repeatedly use.
Embodiment
The present invention will be described further by following examples.
Embodiment 1.
By 500g spherical carbide silicon (diameter 5mm), 500gHZSM-5 spherical catalyst (diameter 5mm, Si/C=20, specific surface area 380m
2/ g) add with mechanical stirring, in three mouthfuls of quartzy bottles of prolong, be placed in microwave cracking instrument, constant power is warming up to 450 DEG C, mechanical stirring 60r/min, add the mud powder of 500g drying and screening gradually, 30min adds complete, continues maintenance 450 DEG C of catalytic pyrolysiss and generates without cut, microwave cracking obtains bio oil 130g, solid residue (soil improvement agent) 271g, GC-MS analyze, and in cracking hydrocarbon oil, arene content reaches and reaches 60.7%.
Embodiment 2.
By 500g spherical carbide silicon (diameter 10mm), 1000gHZSM-5 spherical catalyst (diameter 10mm, Si/C=30, specific surface area 405m
2/ g) add with mechanical stirring, in three mouthfuls of quartzy bottles of prolong, be placed in microwave cracking instrument, constant power is warming up to 550 DEG C, mechanical stirring 60r/min, add the mud powder of 500g drying and screening gradually, 30min adds complete, continues maintenance 550 DEG C of catalytic pyrolysiss and generates without cut, microwave cracking obtains bio oil 136g, solid residue (soil improvement agent) 268g, GC-MS analyze, and in cracking hydrocarbon oil, arene content reaches and reaches 61.8%.
Embodiment 3.
By 500g spherical carbide silicon (diameter 10mm), 500gHZSM-5 spherical catalyst (diameter 10mm, Si/C=30, specific surface area 405m
2/ g) add with mechanical stirring, in three mouthfuls of quartzy bottles of prolong, be placed in microwave cracking instrument, constant power is warming up to 450 DEG C, mechanical stirring 70r/min, add the mud powder of 500g drying and screening gradually, 30min adds complete, continues maintenance 450 DEG C of catalytic pyrolysiss and generates without cut, microwave cracking obtains bio oil 141g, solid residue (soil improvement agent) 265g, GC-MS analyze, and in cracking hydrocarbon oil, arene content reaches and reaches 57.3%.
Embodiment 4.
By 500g spherical carbide silicon (diameter 10mm), 1000gHZSM-5 spherical catalyst (diameter 10mm, Si/C=30, specific surface area 405m
2/ g) add with mechanical stirring, in three mouthfuls of quartzy bottles of prolong, be placed in microwave cracking instrument, constant power is warming up to 600 DEG C, mechanical stirring 80r/min, add the mud powder of 500g drying and screening gradually, 30min adds complete, continues maintenance 600 DEG C of catalytic pyrolysiss and generates without cut, microwave cracking obtains bio oil 132g, solid residue (soil improvement agent) 270g, GC-MS analyze, and in cracking hydrocarbon oil, arene content reaches and reaches 60.2%.
Embodiment 5.
By 500g spherical carbide silicon (diameter 20mm), 1000gHZSM-5 spherical catalyst (diameter 20mm, Si/C=40, specific surface area 450m
2/ g) add with mechanical stirring, in three mouthfuls of quartzy bottles of prolong, be placed in microwave cracking instrument, constant power is warming up to 600 DEG C, mechanical stirring 100r/min, add the mud powder of 500g drying and screening gradually, 30min adds complete, continues maintenance 600 DEG C of catalytic pyrolysiss and generates without cut, microwave cracking obtains bio oil 133g, solid residue (soil improvement agent) 272g, GC-MS analyze, and in cracking hydrocarbon oil, arene content reaches and reaches 58.1%.
Claims (4)
1. micro ware auxiliary catalysis fast pyrogenation mud prepares a method for bio oil and soil improvement agent, it is characterized in that comprising the following steps:
(1) by silicon carbide spheroidal particle: the mass ratio of HZSM-5 spherical catalyst=1:1 ~ 1:2, take silicon carbide spheroidal particle, HZSM-5 spherical catalyst, mix and add in quartz reaction still;
(2) quartz reaction still is placed in microwave cracking instrument, is heated to 450 ~ 600 DEG C, stirring velocity is 60-100r/min, add sludge-drying powder gradually, by the vapor condensation produced, obtain brown liquid product bio oil, and collect solid residue and make soil improvement agent.
2. micro ware auxiliary catalysis fast pyrogenation mud according to claim 1 prepares the method for bio oil and soil improvement agent, it is characterized in that described silicon carbide spherical particle diameters is 5mm-20mm.
3. micro ware auxiliary catalysis fast pyrogenation mud according to claim 1 prepares the method for bio oil and soil improvement agent, it is characterized in that described HZSM-5 spherical catalyst particles diameter is 5mm-20mm, Si/C=20-40, specific surface area 380-450m
2/ g.
4. micro ware auxiliary catalysis fast pyrogenation mud according to claim 1 prepares the method for bio oil and soil improvement agent, it is characterized in that described sludge-drying powder comprises the mud of municipal sewage, by dry 72h at 80 ± 1 DEG C of temperature, after pulverizing, cross 2mm sieve.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948440A (en) * | 2016-07-11 | 2016-09-21 | 许祚员 | Diazinon-polluted sludge treatment agent and preparation method thereof |
| CN105948439A (en) * | 2016-07-11 | 2016-09-21 | 许祚员 | Glyphosate-polluted sludge treatment agent and preparation method |
| CN105967476A (en) * | 2016-07-01 | 2016-09-28 | 苏锦忠 | Carbon tetrachloride contaminated sludge treatment agent and preparation method for same |
| CN106007281A (en) * | 2016-07-11 | 2016-10-12 | 许祚员 | Phenol polluted sludge treatment agent and preparing method thereof |
| CN106082569A (en) * | 2016-07-11 | 2016-11-09 | 许祚员 | A kind of Stam F-34 Contaminated Sewage Sludge inorganic agent and preparation method thereof |
| CN106865939A (en) * | 2017-02-24 | 2017-06-20 | 宜兴市创新环保有限公司 | A kind of oily sludge is quickly granulated pyrolysis system and method |
| CN107652995A (en) * | 2017-11-06 | 2018-02-02 | 南昌大学 | A kind of method that vinasse fast pyrogenation prepares biological flue gas |
| CN107723015A (en) * | 2017-11-06 | 2018-02-23 | 南昌大学 | A kind of device of downdraft fast pyrogenation biomass |
| CN107828431A (en) * | 2017-11-06 | 2018-03-23 | 南昌大学 | A kind of method of the converting fuel oil of shell class discarded object microwave radiation technology |
| CN107892930A (en) * | 2017-11-06 | 2018-04-10 | 南昌大学 | A kind of method of fruit stone class discarded object fast pyrolysis oil production |
| CN108249737A (en) * | 2017-12-26 | 2018-07-06 | 四川建筑职业技术学院 | A kind of method of microwave reinforced catalytic wet oxidation processing sludge |
| CN108439740A (en) * | 2018-05-10 | 2018-08-24 | 南昌大学 | A kind of method of poultry excrement and urine disposal |
| CN109796999A (en) * | 2019-01-31 | 2019-05-24 | 盐城工学院 | A kind of catalytic pyrolysis of biomass method |
| CN112473722A (en) * | 2020-12-11 | 2021-03-12 | 郑州大学 | Biomass charcoal-based characteristic catalyst and method for preparing aromatic hydrocarbon by using same |
| CN114989842A (en) * | 2022-06-09 | 2022-09-02 | 武汉轻工大学 | Method for preparing bio-oil rich in monocyclic aromatic hydrocarbon by biomass graded catalytic pyrolysis |
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| CN1850943A (en) * | 2006-06-02 | 2006-10-25 | 大连理工大学 | Method for preparing biodiesel from sludge by microwave radiation |
| CN101838094A (en) * | 2009-11-13 | 2010-09-22 | 胜利油田胜利工程设计咨询有限责任公司 | Resourceful treatment method and device for oil-containing sludge in oil fields by microwave pyrolysis |
| CN104449789A (en) * | 2014-10-16 | 2015-03-25 | 西安石油大学 | Low-temperature catalytic pyrolysis method for oil-containing sludge |
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| CN1850943A (en) * | 2006-06-02 | 2006-10-25 | 大连理工大学 | Method for preparing biodiesel from sludge by microwave radiation |
| CN101838094A (en) * | 2009-11-13 | 2010-09-22 | 胜利油田胜利工程设计咨询有限责任公司 | Resourceful treatment method and device for oil-containing sludge in oil fields by microwave pyrolysis |
| CN104449789A (en) * | 2014-10-16 | 2015-03-25 | 西安石油大学 | Low-temperature catalytic pyrolysis method for oil-containing sludge |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967476A (en) * | 2016-07-01 | 2016-09-28 | 苏锦忠 | Carbon tetrachloride contaminated sludge treatment agent and preparation method for same |
| CN105948440A (en) * | 2016-07-11 | 2016-09-21 | 许祚员 | Diazinon-polluted sludge treatment agent and preparation method thereof |
| CN105948439A (en) * | 2016-07-11 | 2016-09-21 | 许祚员 | Glyphosate-polluted sludge treatment agent and preparation method |
| CN106007281A (en) * | 2016-07-11 | 2016-10-12 | 许祚员 | Phenol polluted sludge treatment agent and preparing method thereof |
| CN106082569A (en) * | 2016-07-11 | 2016-11-09 | 许祚员 | A kind of Stam F-34 Contaminated Sewage Sludge inorganic agent and preparation method thereof |
| CN106865939A (en) * | 2017-02-24 | 2017-06-20 | 宜兴市创新环保有限公司 | A kind of oily sludge is quickly granulated pyrolysis system and method |
| CN107828431A (en) * | 2017-11-06 | 2018-03-23 | 南昌大学 | A kind of method of the converting fuel oil of shell class discarded object microwave radiation technology |
| CN107723015A (en) * | 2017-11-06 | 2018-02-23 | 南昌大学 | A kind of device of downdraft fast pyrogenation biomass |
| CN107652995A (en) * | 2017-11-06 | 2018-02-02 | 南昌大学 | A kind of method that vinasse fast pyrogenation prepares biological flue gas |
| CN107892930A (en) * | 2017-11-06 | 2018-04-10 | 南昌大学 | A kind of method of fruit stone class discarded object fast pyrolysis oil production |
| CN107652995B (en) * | 2017-11-06 | 2019-10-01 | 南昌大学 | A kind of method that vinasse fast pyrogenation prepares biological flue gas |
| CN107828431B (en) * | 2017-11-06 | 2019-10-01 | 南昌大学 | A kind of method of the microwave-assisted converting fuel oil of shell class waste |
| CN107892930B (en) * | 2017-11-06 | 2019-10-29 | 南昌大学 | A kind of method of fruit stone class waste fast pyrolysis oil production |
| CN108249737A (en) * | 2017-12-26 | 2018-07-06 | 四川建筑职业技术学院 | A kind of method of microwave reinforced catalytic wet oxidation processing sludge |
| CN108439740A (en) * | 2018-05-10 | 2018-08-24 | 南昌大学 | A kind of method of poultry excrement and urine disposal |
| CN108439740B (en) * | 2018-05-10 | 2021-05-07 | 南昌大学 | Method for treating livestock and poultry manure |
| CN109796999A (en) * | 2019-01-31 | 2019-05-24 | 盐城工学院 | A kind of catalytic pyrolysis of biomass method |
| CN112473722A (en) * | 2020-12-11 | 2021-03-12 | 郑州大学 | Biomass charcoal-based characteristic catalyst and method for preparing aromatic hydrocarbon by using same |
| CN114989842A (en) * | 2022-06-09 | 2022-09-02 | 武汉轻工大学 | Method for preparing bio-oil rich in monocyclic aromatic hydrocarbon by biomass graded catalytic pyrolysis |
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