CN112961693A - Method for preparing hydrogen-rich fuel gas by utilizing quick co-pyrolysis of dehydrated Fenton sludge and biomass - Google Patents
Method for preparing hydrogen-rich fuel gas by utilizing quick co-pyrolysis of dehydrated Fenton sludge and biomass Download PDFInfo
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 145
- 239000010802 sludge Substances 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000002028 Biomass Substances 0.000 title claims abstract description 48
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000001257 hydrogen Substances 0.000 title claims abstract description 33
- 239000002737 fuel gas Substances 0.000 title claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 85
- 239000002699 waste material Substances 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 84
- 229910052573 porcelain Inorganic materials 0.000 claims description 36
- 235000010469 Glycine max Nutrition 0.000 claims description 22
- 244000068988 Glycine max Species 0.000 claims description 22
- 239000010902 straw Substances 0.000 claims description 22
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 208000005156 Dehydration Diseases 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- 239000010842 industrial wastewater Substances 0.000 claims 1
- 239000010865 sewage Substances 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052791 calcium Inorganic materials 0.000 abstract description 9
- 239000011575 calcium Substances 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 13
- 239000005416 organic matter Substances 0.000 description 8
- 230000005587 bubbling Effects 0.000 description 7
- 238000005336 cracking Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 238000004817 gas chromatography Methods 0.000 description 5
- 230000004580 weight loss Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 4
- -1 hydroxyl free radical Chemical class 0.000 description 4
- 235000013980 iron oxide Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 230000000630 rising effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- 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
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
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- 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
- C10B57/00—Other carbonising or coking processes; Features of destructive distillation processes in general
- C10B57/08—Non-mechanical pretreatment of the charge, e.g. desulfurization
- C10B57/10—Drying
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/02—Fixed-bed gasification of lump fuel
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/02—Fixed-bed gasification of lump fuel
- C10J3/20—Apparatus; Plants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2200/00—Details of gasification apparatus
- C10J2200/06—Catalysts as integral part of gasifiers
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0913—Carbonaceous raw material
- C10J2300/0916—Biomass
- C10J2300/092—Wood, cellulose
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0983—Additives
- C10J2300/0986—Catalysts
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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
- 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
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- Environmental & Geological Engineering (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a method for preparing hydrogen-rich gas by utilizing quick co-pyrolysis of dehydrated Fenton sludge and biomass, which comprises the steps of mixing dehydrated Fenton sludge powder and biomass waste powder to prepare a pyrolysis precursor raw material; and then taking a proper amount of pyrolysis precursor raw materials, pyrolyzing at 600-800 ℃ under the protection of Ar atmosphere, and collecting the gas-phase product through a gas collecting device. The method is based on the characteristic that the dewatered Fenton sludge contains iron and calcium elements, and the dewatered Fenton sludge is used as a biomass pyrolysis catalyst. The content of hydrogen in biomass pyrolysis gas products can be obviously improved by the dewatered Fenton sludge, and especially the volume percentage of the hydrogen in the combustible gas is obviously improved at the pyrolysis temperature of 800 ℃. The method utilizes the co-pyrolysis of the dewatered Fenton sludge and the biomass to prepare the hydrogen-rich fuel gas, is a good measure for changing waste into valuable and treating waste with waste, and provides an effective way for properly treating the waste and acquiring hydrogen energy.
Description
Technical Field
The invention relates to a method for preparing hydrogen-rich fuel gas by utilizing quick co-pyrolysis of dehydrated Fenton sludge and biomass.
Background
The Fenton oxidation technology is the advanced oxidation technology with the widest application range and the highest use frequency in the current market, and has the characteristics of strong oxidizing property, no selectivity, simple equipment, simple and convenient operation and the like. The Fenton oxidation technology is mainly through Fe2+And H2O2The reaction generates hydroxyl free radical (OH) with strong oxidizing property to realize the oxidative degradation of the pollutants which are difficult to degrade, and after the oxidation process is finished, the iron ions in the water are removed by adding alkali, so that the residual iron ions are separated out in a precipitation form, and the pH value of the wastewater is neutralized. Fenton sludge, i.e. chemical sludge produced during flocculation after the Fenton oxidation process, in which the inorganic material consists mainly of Fe (OH)3And (4) forming. In addition, due to the cheap calcium hydroxide (Ca (OH)2) Or calcium oxide (CaO), is commonly used as an alkaline additive for neutralization and flocculation, and therefore, Fenton sludge generally contains a certain amount of calcium element.
About 5kg of Fenton sludge with the water content of 60 percent is generated when 1 ton of wastewater is treated by using the Fenton oxidation technology, and the Fenton sludge contains various stubborn organic pollutants, heavy metals and sediment impurities, so that the Fenton sludge has dangerous characteristics. The general disposal mode is to bury and burn after concentrating and dehydrating through a plate-and-frame filter press, which causes serious secondary pollution to the environment, and the disposal cost is higher and is about 35-50% of the total operation cost of wastewater treatment. Pyrolysis, one of the most promising thermochemical methods for safely treating sewage sludge, has many advantages over direct treatment methods such as landfill and incineration due to its advantages such as energy recovery, nutrient recycling, heavy metal solidification and high-quality biochar production.
Therefore, based on the background technical content, an environmentally-friendly, economic, green and sustainable Fenton sludge treatment method is found, and is a problem which needs to be solved all over the world at present.
Disclosure of Invention
In summary, aiming at the problems of high yield of dehydrated Fenton sludge, easy secondary pollution caused by improper treatment, high treatment cost and the like in the prior art, the invention aims to provide a method for preparing hydrogen-rich gas by utilizing rapid co-pyrolysis of the dehydrated Fenton sludge and biomass.
The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dewatered Fenton sludge and the biomass is characterized by comprising the following steps of:
1) dewatering the Fenton sludge, grinding the obtained dewatered Fenton sludge, and sieving the ground dewatered Fenton sludge with a 100-mesh sieve to prepare dewatered Fenton sludge powder; drying and crushing the biomass waste, and sieving the crushed biomass waste with a 100-mesh sieve to prepare biomass waste powder;
2) uniformly mixing the dehydrated Fenton sludge powder obtained in the step 1) with biomass waste powder to obtain a pyrolysis precursor raw material;
3) and (3) putting the pyrolysis precursor raw material obtained in the step 2) into Ar atmosphere for pyrolysis, wherein pyrolysis gas generated by pyrolysis is a hydrogen-rich gas product.
The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that in the step 1), the Fenton sludge is precipitated sludge generated by treating waste water containing organic matters by a Fenton process, and contains organic matters and inorganic matters, wherein the main components of the inorganic matters are organic mattersDivided into Fe (OH)3(ii) a In the step 1), the biomass waste is soybean straw.
The method for preparing the hydrogen-rich fuel gas by utilizing the quick co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that in the step 1), the dehydration treatment process of the Fenton sludge is as follows: carrying out primary dehydration on the Fenton sludge through mechanical filter pressing, and drying at the temperature of 100-110 ℃ for 10-20h to obtain dehydrated Fenton sludge;
in the dewatered Fenton sludge, the mass content of organic matters is 25-35%, the mass content of inorganic matters is 60-70%, and the balance is residual moisture;
in the inorganic matter component of the dewatered Fenton sludge, the mass content of ferric oxide is 85-90%, and the mass content of calcium oxide is 1-5%.
The method for preparing the hydrogen-rich gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that in the step 2), the mass ratio of the dehydrated Fenton sludge powder to the biomass waste powder is 0.5-2: 5.
The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that in the step 3), the pyrolysis temperature is 600-850 ℃; the pyrolysis gas produced by pyrolysis contains H2、CO、CH4And CO2Four components, H2、CO、CH4And CO2The total volume fraction of the four components in the pyrolysis gas is more than 85 percent; wherein H2Component (B) is as follows2、CO、CH4And CO2The volume percentage of the four components is more than 40 percent.
The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that the pyrolysis temperature is 800 ℃, and the H in the pyrolysis gas is2Component (B) is as follows2、CO、CH4And CO2The volume percentage of the four components is more than 50 percent.
The method for preparing the hydrogen-rich gas by utilizing the rapid co-pyrolysis of the dewatered Fenton sludge and the biomass is characterized in that a pyrolysis device is adopted in the step 3) to carry out pyrolysis reaction on a pyrolysis precursor raw material, the pyrolysis device comprises a fixed bed reaction tube and a vertical tubular furnace for heating the fixed bed reaction tube, the fixed bed reaction tube is vertically arranged in the vertical tubular furnace, and the upper end of the fixed bed reaction tube penetrates out of the vertical tubular furnace; a porcelain boat with an open upper end is suspended in the fixed bed reaction tube, the porcelain boat is connected to a molybdenum wire, the upper end of the molybdenum wire penetrates out of the top of the fixed bed reaction tube, and the upper and lower positions of the porcelain boat in the fixed bed reaction tube can be adjusted by adjusting the molybdenum wire; wherein, the top of the fixed bed reaction tube is connected with an air inlet pipeline for introducing Ar, and the bottom of the fixed bed reaction tube is connected with a gas collecting device through a pipeline.
The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dewatered Fenton sludge and the biomass is characterized in that the pyrolysis device is adopted to carry out the pyrolysis reaction on the pyrolysis precursor raw material, and the operation steps are as follows:
s1: the pyrolysis precursor raw material is placed in a porcelain boat, the porcelain boat is firstly adjusted to the inner part of the upper end of a fixed bed reaction tube, and the porcelain boat is arranged above the vertical tube furnace; introducing Ar into the fixed bed reaction tube, displacing and exhausting air in the fixed bed reaction tube, and heating the fixed bed reaction tube by a vertical tube furnace;
s2: and (3) when the temperature of the fixed bed reaction tube rises to a set temperature, downwards feeding the porcelain boat into the middle of the fixed bed reaction tube, enabling the porcelain boat to be positioned in a high-temperature section of the fixed bed reaction tube, carrying out pyrolysis under the protection of Ar atmosphere, and collecting gas discharged from the bottom of the fixed bed reaction tube through a gas collecting device to obtain a pyrolysis gas product.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the solid waste dewatered Fenton sludge and the biomass waste soybean straw are used as raw materials for carrying out co-pyrolysis research, and the dewatered Fenton sludge is used for regulating and controlling the distribution of biomass pyrolysis products, so that the yield of biomass pyrolysis gas-phase products is improved, and the available approach of wastes is increased.
2. The method utilizes the characteristic that the dewatered Fenton sludge is rich in iron element to serve as a biomass pyrolysis catalyst, promotes the in-situ catalytic cracking of biomass pyrolysis tar, improves the cracking efficiency of macromolecular organic matters, and increases the yield of micromolecular pyrolysis products.
3. The invention has the advantages of easily obtained raw materials and high product energy density (namely H in gas products)2High content) and less secondary pollution. The invention provides a method for treating wastes with wastes, which reduces the solid wastes and simultaneously provides an effective way for obtaining hydrogen energy while reducing the environmental pollution.
The content of the volatile organic compounds in the dewatered Fenton sludge is low, and high benefit is difficult to obtain by directly carrying out pyrolysis treatment on the dewatered Fenton sludge. In the method, the dewatered Fenton sludge is rich in elements such as iron and calcium with catalytic activity of cracking tar, and can be used as an iron-based and calcium-based catalyst in the pyrolysis process. The redox behavior of the iron element in the pyrolysis process is as follows:
Fe3O4+CO→3FeO+CO2；
3FeO+H2O→Fe3O4+H2。
the calcium cycling reaction is as follows:
the water-vapor transformation reaction comprises the following steps:
in the method, the tar is catalyzed to be converted and the CO in the gas-phase product is absorbed through the oxidation-reduction action of the iron element in the pyrolysis process and the calcium circulation reaction process2Promoting the water-vapor shift reaction towards the generation of H2Is moved. Therefore, the composition of the gas generated by the pyrolysis reaction is changed, and the energy-dense hydrogen-rich gaseous product is obtained.
Therefore, the dewatered Fenton sludge is used as a catalyst and is pyrolyzed together with the biomass waste, so that the quality of a biomass pyrolysis product can be improved, the dewatered Fenton sludge waste can be effectively utilized, the utilization of waste resources is maximized, and the hydrogen-rich fuel gas is obtained. The co-pyrolysis of the dewatered Fenton sludge and the biomass waste is a good measure for changing waste into valuable and treating waste with waste, and an effective way is provided for the proper treatment of the waste and the acquisition of hydrogen energy.
Drawings
FIG. 1 is a schematic view of the pyrolysis apparatus of the present invention;
FIG. 2 is a thermogravimetric experiment result graph of dewatered Fenton sludge;
FIG. 3 shows four target gases H in the pyrolysis gas generated by single pyrolysis of soybean straw under the conditions of pyrolysis temperatures of 600 deg.C, 700 deg.C and 800 deg.C respectively2、CO、CH4And CO2The volume percentage of each component accounts for the ratio result;
FIG. 4 shows four target gases H in the pyrolysis gas generated by the pyrolysis of the dehydrated Fenton sludge and the soybean straw under the conditions that the pyrolysis temperatures are 600 ℃, 700 ℃ and 800 ℃ respectively2、CO、CH4And CO2In the formula (I), the volume percentage of each component accounts for the ratio result.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIG. 1
The schematic structure of the pyrolysis device is shown in fig. 1. The pyrolysis device includes fixed bed reaction tube 2 and is used for carrying out the vertical tube furnace 1 that heats to fixed bed reaction tube 2, and fixed bed reaction tube 2 is vertical to be set up in vertical tube furnace 1, and the upper end of fixed bed reaction tube 2 is worn out vertical tube furnace 1. A porcelain boat 3 with an open upper end is suspended in the fixed bed reaction tube 2, the porcelain boat 3 is connected to a molybdenum wire 4, the upper end of the molybdenum wire 4 penetrates out of the top of the fixed bed reaction tube 2, and the upper and lower positions of the porcelain boat 3 in the fixed bed reaction tube 2 can be adjusted by adjusting the molybdenum wire 4; wherein, the top of the fixed bed reaction tube 2 is connected with an air inlet pipeline for introducing Ar, and the bottom of the fixed bed reaction tube is connected with a gas collecting device through a pipeline.
Wherein, the mode that the porcelain boat 3 is connected with the molybdenum wire 4 can be: the lower extreme of molybdenum filament 4 sets up a plurality of forked connecting wires to through a plurality of forked connecting wires are connected fixedly with the upper end port lateral wall of porcelain boat 3, pull up porcelain boat 3 steadily through a plurality of connecting wires from this, and porcelain boat 3 is located the inside of fixed bed reaction tube 2, and is equipped with the space between porcelain boat 3 and the fixed bed reaction tube 2. The upper end of the molybdenum wire 4 penetrates out of the top of the fixed bed reaction tube 2.
In this application, gas collecting device includes three liquid bubble bottle 5, a filter 6 and an air bag 7, and three liquid bubble bottle 5 connects gradually through the pipeline, and first liquid bubble bottle 5 is connected through pipeline and 2 bottoms of fixed bed reaction tubes, and third liquid bubble bottle 5 is connected by the pipeline through filter 6 and air bag 7, and three liquid bubble bottle 5 is inside all to contain the dichloromethane of certain volume. The gas discharged from the bottom of the fixed bed reaction tube 2 firstly enters the liquid in the first liquid bubbling bottle 5 for bubbling, then sequentially enters the liquid in the second liquid bubbling bottle 5 and the third liquid bubbling bottle 5 for bubbling, and then is collected in the air bag 7 after passing through the filter 6.
The three liquid bubbling bottles 5 are provided in the present invention to facilitate the absorption of components such as tar that are not completely cracked in the gas generated after pyrolysis. In the example methods of the present invention 2-3, Ar was continuously fed into the fixed bed reaction tube 2 to prevent the liquid in the three liquid bubbling bottles 5 from refluxing. Referring to fig. 1, the gas components collected in the gas bag 7 were analyzed by gas chromatography.
Example 1:
the Fenton sludge is dehydrated (the Fenton sludge is from Hangzhou Tai environmental protection science and technology Co., Ltd.), and the treatment process is as follows: the Fenton sludge is firstly subjected to mechanical filter pressing for primary dehydration, and then dried for 12 hours at 105 ℃ to obtain the dehydrated Fenton sludge.
In order to investigate the specific composition of the dewatered Fenton sludge, X-ray fluorescence spectroscopy analysis was performed on the dewatered Fenton sludge to investigate the content of inorganic components therein, and the test results are shown in Table 1.
Table 1 XRF analysis of dewatered Fenton sludge
As can be seen from Table 1, Fe in dewatered Fenton sludge2O3The content of the iron and the iron oxide reaches 89.64 percent, and the iron oxide have very good catalytic activity on tar reforming and cracking reaction, so the dewatered Fenton sludge can be used as an iron-based catalyst in the biomass pyrolysis process. In addition, the CaO content of the dewatered Fenton sludge is 3.65%, and the sludge can absorb CO through calcium circulation in the CO-pyrolysis process2The effect of promoting the water vapor shift reaction in the pyrolysis process to proceed to the hydrogen production direction to obtain more H2。
In order to explore the pyrolysis characteristic of the dehydrated Fenton sludge, a thermogravimetric experiment is carried out on the dehydrated Fenton sludge, and the specific process comprises the following steps: and (3) heating the dewatered Fenton sludge in Ar protective atmosphere, wherein the temperature is increased to 800 ℃ at the temperature rising rate of 10 ℃/min by taking 30 ℃ as an initial temperature. The thermogravimetric experiment result of the dewatered Fenton sludge sample at 30-800 ℃ is shown in figure 2. TG (%) is the proportion of mass loss of the sample with increasing temperature. The curve obtained by the first derivative of the temperature with respect to the DTG (%/min), i.e., the TG curve, is expressed as the weight loss rate of the sample with a gradual rise in the heating temperature by the microperimetric thermogravimetric analysis.
As can be seen from fig. 2: the method comprises the following steps that three main weight loss stages of the dewatered Fenton sludge exist at the temperature of 30-800 ℃, the first stage occurs at the temperature of 30-200 ℃, the first stage is mainly a stage of removing the intramolecular bound water of the dewatered Fenton sludge, the mass loss of the first stage is 8%, the mass residue of a sample is 90%, and the maximum weight loss rate is reached at the temperature of 107 ℃. The second stage is carried out within the range of 200-550 ℃, mainly is the removal and cracking stage of the organic matter volatile matter, the mass loss of the stage is 21%, the mass residue of the sample is 69%, the maximum weight loss rate is reached at 304 ℃, and a wider right shoulder is accompanied, which shows that the volatilization and cracking rate of the organic matter in the dehydrated Fenton sludge is maximum at 304 ℃, and the organic matter is continuously cracked along with the increase of the temperature. The third stage mainly occurs at the temperature higher than 550 ℃, the mass loss in the stage is 7%, the mass of the sample remains 62%, and the temperature of the maximum weight loss peak is 776 ℃, and the third stage is mainly caused by the decomposition of inorganic matters with lower partial thermal stability in the dehydrated Fenton sludge.
The experimental result in fig. 2 shows that the components of the dewatered Fenton sludge are mostly inorganic components except for a small amount of moisture and organic matters, and the weight ratio of the inorganic components is close to 70%. As can be seen from the test results in table 1, the inorganic components in the dewatered Fenton sludge are mainly present as iron oxides.
Because the organic matter volatile matter content in the dewatered Fenton sludge is low, the dewatered Fenton sludge is not suitable for realizing resource utilization in a single pyrolysis mode, and due to the existence of the high iron oxide, the dewatered Fenton sludge and the biomass are endowed with high catalytic activity, the co-pyrolysis can not only make up the deficiency of the organic matter volatile matter content in the raw materials, but also can upgrade the pyrolysis product, and improve the components of hydrogen in the pyrolysis combustible gas.
Example 2:
the pyrolysis device shown in fig. 1 is used for reaction, and in this example, the influence of pyrolysis temperature on the yield of pyrolysis gas and the gas components of soybean straw is explored under the condition that no dehydrated Fenton sludge is added, and the operation process is as follows:
s1: drying and crushing soybean straws, sieving the crushed soybean straws with a 100-mesh sieve to prepare soybean straw powder, and putting 2g of the soybean straw powder in a porcelain boat;
s2: the porcelain boat was first adjusted to the inside of the upper end of the fixed bed reaction tube, and in the comparison fig. 1, the porcelain boat was located above the vertical tube furnace. Continuously introducing Ar with the flow rate of 50mL/min into the fixed bed reaction tube, displacing and exhausting air in the fixed bed reaction tube, and heating the fixed bed reaction tube by using a vertical tube furnace;
s3: and when the temperature of the fixed bed reaction tube rises to the pyrolysis temperature, the porcelain boat is conveyed downwards into the middle part of the fixed bed reaction tube, the porcelain boat is positioned in a high-temperature section of the fixed bed reaction tube, the pyrolysis reaction is started under the protection of Ar atmosphere, the sample in the porcelain boat instantly rises to the target temperature from the room temperature, the organic matter volatile matter in the sample is rapidly separated out, and a large amount of micromolecular gas is generated. The pyrolysis time was 15min, the gas product was collected by an air bag (the air bag started collecting the gas product after the start of the pyrolysis reaction), and the gas composition was detected by gas chromatography.
In the above step S3, the pyrolysis gas yields of the soybean straw at high temperatures are summarized in table 2, with the pyrolysis temperatures set to 600 ℃, 700 ℃, and 800 ℃, respectively.
TABLE 2
In table 2, the yield of pyrolysis gas is the total volume of gas collected by the gas bag within 15min of pyrolysis — the total volume of Ar introduced within 15min of pyrolysis. The yield of four target gases is H in the pyrolysis gas2、CO、CH4And CO2Total volume of four components. The output of combustible gas refers to H in pyrolysis gas2、CO、CH4Total volume of the three components.
As can be seen from table 2: the yield of pyrolysis gas of the soybean straws is gradually increased along with the increase of the temperature, which is mainly caused by that the gradual and thorough cracking reaction of organic matters is gradually intensified along with the increase of the temperature, so that the yield of small molecule gas is increased.
Under the condition that the pyrolysis temperatures are respectively set to be 600 ℃, 700 ℃ and 800 ℃, the pyrolysis gas of the soybean straws at the high temperature is analyzed by gas chromatography, and four target gases (namely H) in the pyrolysis gas2、CO、CH4And CO2) The volume percentage of each component was further analyzed, and the results are summarized in fig. 3. As can be seen from FIG. 3, the major gaseous products in the combustible gas are CO and H at the pyrolysis temperatures of 600 deg.C, 700 deg.C and 800 deg.C2CO and CH4The yield increases with increasing temperature. It can be found that H in four target gases obtained by single pyrolysis of biomass2Low content of H at 800 ℃2The yield ratio was 21%.
Example 3:
the pyrolysis device shown in fig. 1 is used for reaction, and in this example, under the condition of adding the dehydrated Fenton sludge, the influence of the pyrolysis temperature on the yield and the gas components of the pyrolysis gas of the soybean straw is explored, and the operation process is as follows:
s1: the dewatered Fenton sludge obtained in example 1 was ground and sieved with a 100-mesh sieve to obtain dewatered Fenton sludge powder. Drying and crushing the soybean straws, and sieving the crushed soybean straws with a 100-mesh sieve to prepare soybean straw powder.
S2: and (5) uniformly mixing the dewatered Fenton sludge powder obtained in the step (S1) and the soybean straw powder according to the mass ratio of 1:5 to obtain mixed powder. 2g of the mixed powder was placed in a porcelain boat.
S2: the porcelain boat was first adjusted to the inside of the upper end of the fixed bed reaction tube, and in the comparison fig. 1, the porcelain boat was located above the vertical tube furnace. Continuously introducing Ar with the flow rate of 50mL/min into the fixed bed reaction tube, displacing and exhausting air in the fixed bed reaction tube, and heating the fixed bed reaction tube by using a vertical tube furnace;
s3: when the temperature of the fixed bed reaction tube rises to the pyrolysis temperature, the porcelain boat is conveyed downwards to the inner part of the middle part of the fixed bed reaction tube, the porcelain boat is positioned in a high-temperature section of the fixed bed reaction tube, the pyrolysis reaction is started under the protection of Ar atmosphere, a sample in the porcelain boat instantly rises from room temperature to a target temperature, the volatile matter of the organic matter of the sample is rapidly separated out, the volatile matter is analyzed and simultaneously reacts with iron and calcium elements in the dehydrated Fenton sludge, a macromolecular organic product is continuously cracked after iron catalysis to generate a large amount of micromolecular gas, and CO in the micromolecular gas2After calcium circulation absorption, the H in the pyrolysis gas phase product is promoted2The content is greatly increased. The pyrolysis time was 15min, the gas product was collected by an air bag (the air bag started collecting the gas product after the start of the pyrolysis reaction), and the gas composition was detected by gas chromatography.
In the above step S3, the pyrolysis gas yields of the soybean straw at high temperatures are summarized in table 3, in the case where the pyrolysis temperatures are set to 600 ℃, 700 ℃, and 800 ℃, respectively.
TABLE 3
In table 3, the yield of pyrolysis gas is the total volume of gas collected by the gas bag within 15min of pyrolysis — the total volume of Ar introduced within 15min of pyrolysis. The yield of four target gases is H in the pyrolysis gas2、CO、CH4And CO2Total volume of four components. The output of combustible gas refers to H in pyrolysis gas2、CO、CH4Total volume of the three components.
As can be seen from table 3: along with the increase of the temperature, the yield of pyrolysis gas of the dehydrated Fenton sludge and the soybean straws is gradually increased, which is mainly caused by that along with the increase of the temperature, organic matters are gradually and completely cracked, the reaction is gradually intensified, and the yield of small molecule gas is increased.
Setting pyrolysis temperatures to be 600 ℃, 700 ℃ and 800 ℃, respectively, and analyzing pyrolysis gas of the dehydrated Fenton sludge and the soybean straws at the high temperature through gas chromatography, wherein the pyrolysis gas is aimed at four target gases (namely H) in the pyrolysis gas2、CO、CH4And CO2) The volume percentage of each component was further analyzed, and the results are summarized in fig. 4.
As can be seen in fig. 4: at the pyrolysis temperature of 600 ℃, 700 ℃ and 800 ℃, the main gas product components in the combustible gas are obviously changed, and the main gas product is converted from CO into H2And H in the four target gases2The volume ratio is more than 40 percent. The substances with catalytic activity such as iron, calcium and the like in the dehydrated Fenton sludge are probably substances with catalytic activity, the reaction path of organic matter cracking is changed in the pyrolysis process, the aromatization of pyrolysis products is accelerated, the dehydrogenation reaction is promoted, and therefore H in gaseous products is caused2The content is obviously increased. These results further demonstrate that the dewatered Fenton sludge plays a catalytic role in the pyrolysis process of the soybean straw powder.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (8)
1. A method for preparing hydrogen-rich fuel gas by utilizing the fast co-pyrolysis of dehydrated Fenton sludge and biomass is characterized by comprising the following steps:
1) dewatering the Fenton sludge, grinding the obtained dewatered Fenton sludge, and sieving the ground dewatered Fenton sludge with a 100-mesh sieve to prepare dewatered Fenton sludge powder; drying and crushing the biomass waste, and sieving the crushed biomass waste with a 100-mesh sieve to prepare biomass waste powder;
2) uniformly mixing the dehydrated Fenton sludge powder obtained in the step 1) with biomass waste powder to obtain a pyrolysis precursor raw material;
3) and (3) putting the pyrolysis precursor raw material obtained in the step 2) into Ar atmosphere for pyrolysis, wherein pyrolysis gas generated by pyrolysis is a hydrogen-rich gas product.
2. The method for preparing hydrogen-rich fuel gas by fast co-pyrolysis of dewatered Fenton sludge and biomass as claimed in claim 1, wherein in step 1), the Fenton sludge is precipitated sludge generated by Fenton process treatment of municipal sewage and industrial wastewater, and comprises organic matters and inorganic matters, wherein the main component of the inorganic matters is Fe (OH)3(ii) a In the step 1), the biomass waste is soybean straw.
3. The method for preparing the hydrogen-rich fuel gas by utilizing the fast co-pyrolysis of the dewatered Fenton sludge and the biomass as claimed in claim 1, wherein in the step 1), the dewatering treatment process of the Fenton sludge comprises the following steps: carrying out primary dehydration on the Fenton sludge through mechanical filter pressing, and drying at the temperature of 100 ℃ and 110 ℃ for 10-20h to obtain dehydrated Fenton sludge;
in the dewatered Fenton sludge, the mass content of organic matters is 25-35%, the mass content of inorganic matters is 60-70%, and the balance is residual moisture;
in the inorganic matter component of the dewatered Fenton sludge, the mass content of ferric oxide is 85-90%, and the mass content of calcium oxide is 1-5%.
4. The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass as claimed in claim 1, wherein in the step 2), the mass ratio of the dehydrated Fenton sludge powder to the biomass waste powder is 0.5-2.0: 5.0.
5. The method for preparing hydrogen-rich fuel gas by fast co-pyrolysis of dewatered Fenton sludge and biomass according to claim 1, wherein in step 3), a pyrolysis device is used for carrying out pyrolysis reaction on a pyrolysis precursor raw material, the pyrolysis device comprises a fixed bed reaction tube and a vertical tube furnace for heating the fixed bed reaction tube, the fixed bed reaction tube is vertically arranged in the vertical tube furnace, and the upper end of the fixed bed reaction tube penetrates out of the vertical tube furnace; a porcelain boat with an open upper end is suspended in the fixed bed reaction tube, the porcelain boat is connected to a molybdenum wire, the upper end of the molybdenum wire penetrates out of the top of the fixed bed reaction tube, and the upper and lower positions of the porcelain boat in the fixed bed reaction tube can be adjusted by adjusting the molybdenum wire; wherein, the top of the fixed bed reaction tube is connected with an air inlet pipeline for introducing Ar, and the bottom of the fixed bed reaction tube is connected with a gas collecting device through a pipeline.
6. The method for preparing hydrogen-rich fuel gas by fast co-pyrolysis of dewatered Fenton sludge and biomass according to claim 5, wherein the pyrolysis reaction of the pyrolysis precursor raw material by the pyrolysis device comprises the following steps:
s1: the pyrolysis precursor raw material is placed in a porcelain boat, and the porcelain boat is firstly adjusted to the inner part of the upper end of a fixed bed reaction tube, so that the porcelain boat is arranged above the vertical tube furnace; introducing Ar into the fixed bed reaction tube, displacing and exhausting air in the fixed bed reaction tube, and heating the fixed bed reaction tube by a vertical tube furnace;
s2: and (3) when the temperature of the fixed bed reaction tube rises to a set temperature, downwards feeding the porcelain boat into the middle of the fixed bed reaction tube, enabling the porcelain boat to be positioned in a high-temperature section of the fixed bed reaction tube, carrying out pyrolysis under the protection of Ar atmosphere, and collecting gas discharged from the bottom of the fixed bed reaction tube through a gas collecting device to obtain a pyrolysis gas product.
7. The method of claim 1The method for preparing the hydrogen-rich fuel gas by utilizing the rapid co-pyrolysis of the dehydrated Fenton sludge and the biomass is characterized in that in the step 3), the pyrolysis temperature is 600-850 ℃; the pyrolysis gas produced by pyrolysis contains H2、CO、CH4And CO2Four components, the total volume fraction of which in the pyrolysis gas is more than 85%; wherein H2Component (B) is as follows2、CO、CH4And CO2The volume percentage of the four components is more than 40 percent.
8. The method for preparing hydrogen-rich fuel gas by fast co-pyrolysis of dewatered Fenton sludge and biomass as claimed in claim 7, wherein the pyrolysis temperature is 800 ℃, and the H in the pyrolysis gas is2Component (B) is as follows2、CO、CH4And CO2The volume percentage of the four components is more than 50 percent.
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