CN112047436A - Method for preparing micro-electrolysis filler from oil sludge pyrolysis residue and application thereof - Google Patents
Method for preparing micro-electrolysis filler from oil sludge pyrolysis residue and application thereof Download PDFInfo
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- CN112047436A CN112047436A CN202010850711.3A CN202010850711A CN112047436A CN 112047436 A CN112047436 A CN 112047436A CN 202010850711 A CN202010850711 A CN 202010850711A CN 112047436 A CN112047436 A CN 112047436A
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- oil sludge
- pyrolysis residue
- sludge pyrolysis
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- filler
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46176—Galvanic cells
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a method for preparing a micro-electrolysis filler by using oil sludge pyrolysis residues and application thereof, wherein the micro-electrolysis filler is prepared by using impurities such as residual coke, heavy oil and the like in the oil sludge pyrolysis residues as a carbon source and heavy metals such as residual iron and the like as an iron source, is used for treating high-concentration organic wastewater, particularly oily wastewater, plays a role in treating pollution by using pollution, and provides a new way for resource utilization of the oil sludge pyrolysis residues.
Description
The technical field is as follows:
the invention relates to a method for regenerating pyrolysis residues and application thereof, in particular to a method for preparing a micro-electrolysis filler from oil sludge pyrolysis residues and application thereof.
Background art:
the oil sludge pyrolysis residue is solid waste residue generated after oil-containing sludge or distilled oil residue is subjected to high-temperature pyrolysis treatment, the residue is listed in national hazardous waste records, and secondary pollution can be caused if the residue is not properly treated. At present, the research on the pyrolysis of oil sludge at home and abroad mainly focuses on the research on the pyrolysis process and the analysis of gas, solid and liquid products generated in the pyrolysis. The residue in the oil-containing sludge pyrolysis product accounts for a large proportion, and the residue contains incompletely recycled oil resources, residual heavy metal elements and the like, so that if the residue is simply buried, not only can the resources be wasted, but also the environment can be seriously polluted secondarily.
The earlier research results of the subject group refer to CN111482176A, and the method discloses a method for recycling oil sludge pyrolysis residues, wherein metal elements such as iron and aluminum in the oil sludge pyrolysis residues and silicon are used for preparing a nano-scale catalyst, and the nano-scale catalyst is circularly applied to oil sludge pyrolysis, so that the purpose of changing waste into valuable is achieved, secondary pollution of hazardous waste is avoided, and the method has important practical significance for enterprises to carry out clean production, save resources and develop circular economy.
The invention content is as follows:
the invention aims to provide a method for preparing a micro-electrolysis filler from oil sludge pyrolysis residues and application thereof, wherein the micro-electrolysis iron-carbon filler is prepared by using impurities such as residual coke, heavy oil and the like in the oil sludge pyrolysis residues as carbon sources and heavy metals such as residual iron and the like as iron sources, is used for treating high-concentration organic wastewater, particularly oily wastewater, has the effect of treating waste by waste, and provides a new way for resource utilization of the oil sludge pyrolysis residues.
The invention is realized by the following technical scheme:
the method for preparing the micro-electrolysis filler from the oil sludge pyrolysis residue comprises the following steps:
1) crushing the oil sludge pyrolysis residue which is not pretreated or is pretreated, preferably to 130-160 mu m, most preferably to 150 mu m, uniformly mixing the crushed residue with reduced iron powder and high clay with the viscosity of more than or equal to 150 mpa.S, adding water accounting for 18-22 percent of the total weight of the mixture, molding the mixture by using a briquette ball press, and roasting the mixture in a 300-600 ℃ sintering furnace for 1-4 hours to prepare the micro-electrolysis filler;
the pretreatment comprises the following steps: soaking the oil sludge pyrolysis residue in alkali liquor for 6-48h, filtering, placing a filter cake in a tubular furnace, heating to 300-500 ℃ under the protection of nitrogen, carbonizing at constant temperature for 0.5-2 h, switching to 500-850 ℃ under the protection of hydrogen, and reducing at constant temperature for 0.5-2 h to obtain pretreated oil sludge pyrolysis residue; the alkali liquor is one or a mixture of sodium hydroxide and potassium hydroxide, the mass percentage concentration of the alkali liquor is 5-20%, and the mass ratio of the alkali liquor to the oil sludge pyrolysis residue is 2-10.
The oil sludge pyrolysis residue is pyrolysis residue obtained after dehydration and pyrolysis of oil sludge, and comprises main components of iron element, carbon element, calcium element, and metal elements such as aluminum, copper, nickel, zinc, titanium and the like, wherein the mass fraction of the iron element is more than or equal to 10%, the mass fraction of the carbon element is more than or equal to 13%, and the mass fraction of the calcium element is more than or equal to 8%.
The mass fraction of iron in the micro-electrolysis filler is 30-60%, and the mass fraction of high clay is 10-35%; the high clay is one of attapulgite, bentonite, sepiolite and other high clays.
The obtained micro-electrolysis filler is used for treating high-concentration organic wastewater with COD of more than 2000mg/L, in particular oily wastewater.
The invention has the following beneficial effects:
(1) the micro-electrolysis filler is prepared by utilizing impurities such as residual coke, heavy oil, iron and the like in the oil sludge pyrolysis residue, so that the problem of environmental pollution of the oil sludge pyrolysis residue is solved, and the micro-electrolysis filler with higher added value is prepared, so that waste is changed into valuable.
(2) The micro-electrolysis filler prepared from the reductive iron powder and the high clay is supplemented by taking the oil sludge pyrolysis residue or the pretreated oil sludge pyrolysis residue as a raw material, is used for treating high-concentration organic wastewater, particularly oily wastewater, plays a role in treating waste by waste, and provides a new way for resource utilization of the oil sludge pyrolysis residue.
(3) The method has the advantages of simple process, low operation cost, easy industrialization and important economic value and practical significance.
The specific implementation mode is as follows:
the following is a further description of the invention and is not intended to be limiting.
Example 1:
100.00g of the oil sludge pyrolysis residue which is crushed to 150 mu m and is not pretreated is taken, 134.00g of reduced iron powder and 66.00g of attapulgite clay are added and mixed evenly, 60.00g of water is added and then the mixture is molded by a briquette ball press, and the mixture is roasted for 2.0h in a sintering furnace at 350 ℃ to prepare the micro-electrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 8730.00mg/L, and the removal rate of petroleum substances is 68 percent.
Example 2:
soaking 500.00g of oil sludge pyrolysis residue in 1000.00g of 20% sodium hydroxide solution for 6.0h, filtering, placing a filter cake in a tubular furnace, heating to 300 ℃ under the protection of nitrogen, carbonizing for 2.0h at constant temperature, switching to 500 ℃ under the protection of hydrogen, and reducing for 2.0h at constant temperature to obtain pretreated oil sludge pyrolysis residue; pulverizing to 150 μm, collecting 100.00g, adding 134.00g reduced iron powder and 66.00g attapulgite clay, mixing, adding 60.00g water, molding with briquette ball press, and calcining in 350 deg.C sintering furnace for 2.0 hr to obtain microelectrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 12860.00mg/L, and the removal rate of petroleum substances is 79%.
Example 3:
placing 500.00g of oil sludge pyrolysis residue in 2000.00g of potassium hydroxide solution with the mass fraction of 15% to be soaked for 12.0h, then filtering, placing a filter cake in a tubular furnace, heating to 350 ℃ under the protection of nitrogen, carbonizing at constant temperature for 1.5h, switching to 600 ℃ under the protection of hydrogen, and reducing at constant temperature for 1.5h to obtain pretreated oil sludge pyrolysis residue; pulverizing to 150 μm, collecting 100.00g, adding reduced iron powder 95.00g and bentonite clay 105.00g, mixing, adding water 60.00g, molding with briquette ball press, and calcining in 300 deg.C sintering furnace for 4.0 hr to obtain microelectrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 13580.00mg/L, and the removal rate of petroleum substances is 82%.
Example 4:
soaking 500.00g of oil sludge pyrolysis residue in 3000.00g of a mixed solution (mass ratio is 2:1) of sodium hydroxide and potassium hydroxide with the mass fraction of 10% for 24 hours, filtering, placing a filter cake in a tubular furnace, heating to 500 ℃ under the protection of nitrogen, carbonizing at constant temperature for 1.0 hour, switching to 700 ℃ under the protection of hydrogen, and reducing at constant temperature for 1.0 hour to obtain pretreated oil sludge pyrolysis residue; pulverizing to 150 μm, collecting 100.00g, adding 140.00g reduced iron powder and 60.00g attapulgite clay, mixing, adding 60.00g water, molding with briquette ball press, and calcining in 400 deg.C sintering furnace for 2.0h to obtain microelectrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 15770.00mg/L, and the removal rate of petroleum substances is 88 percent.
Example 5:
soaking 500g of oil sludge pyrolysis residue in 4000g of 5% sodium hydroxide and potassium hydroxide mixed solution (mass ratio is 2:1) for 48 hours, filtering, placing a filter cake in a tubular furnace, heating to 450 ℃ under the protection of nitrogen, carbonizing at constant temperature for 0.5 hour, switching to 800 ℃ under the protection of hydrogen, and reducing at constant temperature for 0.5 hour to obtain pretreated oil sludge pyrolysis residue; crushing the materials to 150 mu m, taking 100.00g, adding 110.00g of reduced iron powder and 90.00g of sepiolite high clay, uniformly mixing all the materials, adding 60.00g of water, molding by using a briquette ball press machine, and roasting in a sintering furnace at 600 ℃ for 1.0h to obtain the micro-electrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 11996.00mg/L, and the removal rate of petroleum substances is 75 percent.
Example 6:
soaking 500g of oil sludge pyrolysis residue in 5000g of 10% potassium hydroxide solution by mass for 30h, filtering, placing a filter cake in a tubular furnace, heating to 400 ℃ under the protection of nitrogen, carbonizing at constant temperature for 2.0h, switching to 850 ℃ under the protection of hydrogen, and reducing at constant temperature for 0.5h to obtain pretreated oil sludge pyrolysis residue; pulverizing to 150 μm, collecting 100.00g, adding 170.00g reduced iron powder and 30.00g attapulgite clay, mixing, adding 60.00g water, molding with briquette ball press, and calcining in 500 deg.C sintering furnace for 1.5 hr to obtain microelectrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 14698.00mg/L, and the removal rate of petroleum substances is 85 percent.
Example 7:
soaking 500g of oil sludge pyrolysis residue in 2500g of mixed solution (mass ratio is 2:1) of sodium hydroxide and potassium hydroxide with mass fraction of 16% for 18h, filtering, placing a filter cake in a tubular furnace, heating to 450 ℃ under the protection of nitrogen, carbonizing at constant temperature for 2.0h, switching to 800 ℃ under the protection of hydrogen, and reducing at constant temperature for 1.0h to obtain pretreated oil sludge pyrolysis residue; pulverizing to 150 μm, collecting 100.00g, adding 147.50g reduced iron powder and 52.50g attapulgite clay, mixing, adding 60.00g water, molding with briquette ball press, and calcining in sintering furnace at 450 deg.C for 2.5 hr to obtain microelectrolysis filler.
After the oily wastewater is treated by the micro-electrolysis iron-carbon filler, the COD is reduced by about 16679.00mg/L, and the removal rate of petroleum substances is 89%.
The technical solution of the present invention is not limited to the above embodiments, and other embodiments obtained according to the technical solution of the present invention should fall within the protection scope of the present invention.
Claims (7)
1. The method for preparing the micro-electrolysis filler from the oil sludge pyrolysis residue is characterized by comprising the following steps of:
crushing the oil sludge pyrolysis residue which is not pretreated or is pretreated, uniformly mixing the crushed oil sludge pyrolysis residue with reduced iron powder and high clay with the viscosity of more than or equal to 150 mpa.S, adding water accounting for 18-22% of the total weight of a solid, forming the mixture by using a briquette ball press, and roasting the mixture for 1-4 hours in a sintering furnace at the temperature of 300-600 ℃ to prepare the micro-electrolysis filler;
the pretreatment comprises the following steps: soaking the oil sludge pyrolysis residue in alkali liquor for 6-48h, filtering, placing a filter cake in a tubular furnace, heating to 300-500 ℃ under the protection of nitrogen, carbonizing at constant temperature for 0.5-2 h, switching to 500-850 ℃ under the protection of hydrogen, and reducing at constant temperature for 0.5-2 h to obtain pretreated oil sludge pyrolysis residue; the alkali liquor is one or a mixture of sodium hydroxide and potassium hydroxide, the mass percentage concentration of the alkali liquor is 5-20%, and the mass ratio of the alkali liquor to the oil sludge pyrolysis residue is 2-10.
2. The method for preparing the micro-electrolysis filler from the oil sludge pyrolysis residue as claimed in claim 1, wherein the mass fraction of iron in the micro-electrolysis filler is 30-60%, and the mass fraction of high clay in the micro-electrolysis filler is 10-35%; the high clay is one of attapulgite, bentonite and sepiolite.
3. The method for preparing the micro-electrolysis filler from the oil sludge pyrolysis residue according to claim 1, wherein the oil sludge pyrolysis residue is pyrolysis residue obtained after dehydration and pyrolysis of oil sludge, and comprises iron, carbon and calcium as main components, and also comprises aluminum, copper, nickel, zinc and titanium, wherein the mass fraction of the iron is more than or equal to 10%, the mass fraction of the carbon is more than or equal to 13% and the mass fraction of the calcium is more than or equal to 8%.
4. The method for preparing micro-electrolytic filler from oil sludge pyrolysis residue as claimed in claim 1, wherein the oil sludge pyrolysis residue without pretreatment or after pretreatment is crushed to 130-160 μm.
5. The process for preparing a micro-electrolytic filler from sludge pyrolysis residue according to claim 1, characterized in that the sludge pyrolysis residue without or after pretreatment is crushed to 150 μm.
6. Use of the microelectrolytic filler obtained according to the process of claim 1, characterized in that it is used for the treatment of high-concentration organic waste waters with a COD of above 2000 mg/L.
7. Use according to claim 6, for the treatment of oily wastewater.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010850711.3A CN112047436A (en) | 2020-08-21 | 2020-08-21 | Method for preparing micro-electrolysis filler from oil sludge pyrolysis residue and application thereof |
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| CN202010850711.3A CN112047436A (en) | 2020-08-21 | 2020-08-21 | Method for preparing micro-electrolysis filler from oil sludge pyrolysis residue and application thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874997A (en) * | 2011-07-11 | 2013-01-16 | 中国石油化工股份有限公司 | Oil-containing sludge pyrolysis and its resource treatment method |
| CN105502588A (en) * | 2015-11-26 | 2016-04-20 | 中国科学院广州能源研究所 | Iron-carbon filler pretreated by micro-electrolysis of industrial wastewater and preparation method thereof |
| CN107935129A (en) * | 2018-01-10 | 2018-04-20 | 南华大学 | A kind of preparation method of iron sludge base biology carbon micro-electrolysis filler and its application in uranium-containing waste water is handled |
| CN109911990A (en) * | 2019-03-04 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of preparation method of highly active Fe carbon micro-electrolysis filler |
| CN110451754A (en) * | 2019-07-30 | 2019-11-15 | 中国科学院过程工程研究所 | A kind of method for innocent treatment of greasy filth pyrolysis |
| CN111482176A (en) * | 2020-04-26 | 2020-08-04 | 江苏森茂能源发展有限公司 | Method for recycling oil sludge pyrolysis residues |
-
2020
- 2020-08-21 CN CN202010850711.3A patent/CN112047436A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874997A (en) * | 2011-07-11 | 2013-01-16 | 中国石油化工股份有限公司 | Oil-containing sludge pyrolysis and its resource treatment method |
| CN105502588A (en) * | 2015-11-26 | 2016-04-20 | 中国科学院广州能源研究所 | Iron-carbon filler pretreated by micro-electrolysis of industrial wastewater and preparation method thereof |
| CN107935129A (en) * | 2018-01-10 | 2018-04-20 | 南华大学 | A kind of preparation method of iron sludge base biology carbon micro-electrolysis filler and its application in uranium-containing waste water is handled |
| CN109911990A (en) * | 2019-03-04 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of preparation method of highly active Fe carbon micro-electrolysis filler |
| CN110451754A (en) * | 2019-07-30 | 2019-11-15 | 中国科学院过程工程研究所 | A kind of method for innocent treatment of greasy filth pyrolysis |
| CN111482176A (en) * | 2020-04-26 | 2020-08-04 | 江苏森茂能源发展有限公司 | Method for recycling oil sludge pyrolysis residues |
Non-Patent Citations (2)
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