CN102849905B - Experimental method of oil-containing sludge heat treatment - Google Patents
Experimental method of oil-containing sludge heat treatment Download PDFInfo
- Publication number
- CN102849905B CN102849905B CN201210078373.1A CN201210078373A CN102849905B CN 102849905 B CN102849905 B CN 102849905B CN 201210078373 A CN201210078373 A CN 201210078373A CN 102849905 B CN102849905 B CN 102849905B
- Authority
- CN
- China
- Prior art keywords
- oil
- oily sludge
- temperature
- treatment
- containing sludge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
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
- 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
- Treatment Of Sludge (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
An experimental method of oil-containing sludge heat treatment is applicable to research of oil-containing sludge heat treatment effect and characteristics. The programmed heating process comprises the following steps of: firstly, desiccation treatment, wherein an oil-containing sludge sample is heated from room temperature to 200-250 DEG C to realize complete moisture evaporation, and the composition of non-condensable gas and recovered oil is analyzed; secondly, pyrolysis treatment, wherein the desiccated oil sludge is heated to 600-700 DEG C to realize complete pyrolysis of organic substances such as heavy oil, asphaltene and the like in the oil sludge by high-temperature heating, and the composition of recovered oil and non-condensable gas is analyzed; thirdly, calcination treatment, wherein the oil-containing sludge pyrolytic residues are heated to 800-900 DEG C, and the content of pollutants such as petroleum and the like is analyzed. The method is convenient and rapid for the obtaining of the yield and composition data of heat treatment products of the oil-containing sludge at different heating temperature phases, and for the research and mastering of the heat treatment effect and characteristics of oil-containing sludge, and can realize the purpose of harmless and resource utilization of oil-containing sludge.
Description
Technical field
The present invention relates to oil, petrochemical industry field of environment protection, is the heat treated experimental technique of a kind of oily sludge.The method is applicable to experimental evaluation and the technical study that oil field refinery is produced minimizing, resource utilization and the harmless treatment of the refuses such as oily sludge that produce with Sewage treatment systems.
Background technology
Oily sludge is the solid waste producing in oil production and refining process, except containing petroleum substance, also contains the hazardous and noxious substances such as benzene, phenols, is put into " national Hazardous Waste List " management.Along with the increase of oil production with oil refining scale, the quantity that oily sludge produces is more and more, to the harm of environment, pollute more and more serious.Therefore, carry out from oily sludge refiltered oil, realize the research of residue harmlessness disposing, the environment challenge facing solving the energy shortage problem of Chinese national economy sustainable development process is significant.
At present, oily sludge recycling treatment technology can be divided into: physical chemistry transformation technology and thermal transition technology.Wherein, material chemical treatment method, such as extracting process, hot water wash method, is only applicable to oleaginousness at more than 5～10% oily sludges, and need adds chemical agent, still has sewage, waste sludge discharge, and processing costs is higher.Thermal transition technology, such as burning disposal with make fuel, brickmaking technology, although can process thoroughly the harmful poisonous organism in oily sludge, but need set up incinerator, add combustion-supporting fuel simultaneously, have exhaust gas emission, can not reclaim the crude oil in oily sludge, there is exhaust gas emission, also easily secondary pollution.In all multi-methods, pyrolytic technique is not only conducive to improve the oil recovery rate of oily sludge, and part heavy bitumen material can coking become solid carbon under comparatively high temps, solidifies in oily sludge the objectionable impuritiess such as heavy metal, realizes the innoxious of pyrolysis residue.Therefore, the research of oily sludge pyrolytic technique is more and more subject to people's attention.
Pyrolytic technique can be divided into two kinds of the thermal radiation heating of traditional heat source and microwave heating pyrolysis.Microwave, as a kind of emerging technology, is different from traditional heating mode, and it is that the body that material is caused by dielectric loss at elect magnetic field heats, and its energy transmits with hertzian wave form by space or medium.With the hot thermal radiation of traditional heat source heating relatively, microwave have homogeneous heating, efficient fast, be easy to control to and material is had selectivity, has the features such as katalysis.Although there is the report that adopts microwave-heating technical finesse oily sludge, its main purpose is using the residue process modification after oily sludge pyrolysis as sorbing material.Microwave has the obvious characteristics such as wavelength short (1～1mm) frequency high (300～300GHZ), Quantum Properties.People are applied to stationery, timber, the physical refining process such as resin extruded by microwave heating technique.Not only can effectively improve reaction conversion ratio, and embody the plurality of advantages such as energy-conserving and environment-protective.
Patent ZL200610103671.6 has proposed " a kind of recycling processing method of oily sludge ", soon oily sludge is sent in airtight carbonization decomposition stove or horizontal rotation gas retort and is carried out pyrolysis processing, pyrolysis processing is reacted 1～5 hour under 200～600 ℃ of conditions, refiltered oil air water cut and pyrolysis residue.It is characterized in that pyrolysis processing temperature is 500～600 ℃, the pyrolysis processing reaction times is 2～3 hours, and the pyrolytic reaction time of the method is long, this will cause treatment facility scale large, invest highly, power consumption and the cost of operation are high.Publication CN101838094A, " a kind of Sludge in Oilfields microwave-heating recycling processing method and device " is provided, oily sludge is sent in the closed reactor of microwave heating, at 200～900 ℃ of temperature, carry out pyrolysis processing, the oil gas water that pyrolysis processing is produced carries out recycling, residue after pyrolysis is made roadbed material or is utilized nitric acid or utilize NaOH alkali to carry out modification, and the residue after modification is done sorbing material.The method remains only have been considered and can carry out the net result that the temperature range of pyrolysis and product reclaim, and cannot obtain oily sludge at the generation of the heat-treated products of different heating temperature section and form data, can not study heat treatment process feature and the effect of grasping oily sludge.
Summary of the invention:
The object of the invention is to: for a kind of the provide environment protection of the innoxious experimental technique ，Wei oil field refinery production process with resource utilization of reliable, the efficient oily sludge easily of science and the support that cleaner production provides scientific research basic methods are provided for the oily sludge Pollution abatement of petroleum and petrochemical industry.
The inventive method is achieved in that the heat treated experimental technique of oily sludge is that oily sludge sample is inserted in microwave heating reactor, adopt temperature-programmed mode to carry out heat treated to oily sludge, by to the generation of heat-treated products and compositional analysis, to study the heat treated feature of oily sludge and effect.Its Temperature Programmed Processes is:
The first step, drying and other treatment.Oily sludge sample is elevated to 200～250 ℃ from room temperature, moisture is evaporated completely, complete the drying and other treatment of oily sludge, its cut carries out condensation separation, measures respectively the generation of non-condensable gas, refiltered oil and recycle-water, analyzes non-condensable gas and reclaims oil composition.
Second step, pyrolysis processing.Again mummification greasy filth temperature is elevated to 600～700 ℃, make in greasy filth the organic substance such as heavy oil, bituminous matter carry out complete cracking because of high-temperature heating, complete the pyrolysis processing of mummification greasy filth, its cut carries out condensation separation, measure respectively the generation of non-condensable gas, refiltered oil and recycle-water, analyze the composition of refiltered oil and non-condensable gas.
The 3rd step, calcination is processed.Oily sludge pyrolysis residue temperature is elevated to 800～900 ℃, makes the complete coking of pyrolysis residue, the calcination that completes pyrolysis residue is processed, and the bright residue of heat takes out and weighs after being cooled to room temperature, analyzes the content of the pollutents such as petroleum-type.
Microwave heating reactor volume is 1000～5000ml, and the best is 2000～3000ml.
The sample amount of inserting of Pyrolysis Experiment is 1000～3000g, and the best is 1000～2000g.
It is 10～60 ℃/min that drying and other treatment is controlled temperature rise rate, and top temperature is 200～250 ℃.
It is 50～80 ℃/min that pyrolysis processing is controlled temperature rise rate, 600～700 ℃ of top temperatures.
Calcination processing controls temperature rise rate is 70～100 ℃/min, 800～900 ℃ of top temperatures.
Drying and other treatment, pyrolysis processing and calcination are processed the high temperature cut producing and are carried out independent condensation separation, respectively non-condensable gas, refiltered oil and recycle-water are measured, and respectively non-condensable gas and refiltered oil are sampled to detection.
Beneficial effect of the present invention: the present invention utilizes microwave heating technique, moisture according to oily sludge height, form complicated feature, adopt temperature programming mould to carry out heat treated to sample, by generation and the compositional analysis of the heat-treated products in different heating section, can effectively understand moisture and the heating volatilization of oil component and the situation of decomposition in oily sludge, thermal effectiveness and the feature of oily sludge grasped in research comprehensively, can be the exploitation of oily sludge heat treatment technics, appliance arrangement development and engineering design provide the reliable laboratory facilities of science and important foundation experimental data.Adopt microwave heating to process the oily sludge of oil field Petrochemical Enterprises, not only can reduce the pollution of oily sludge to environment, and be conducive to recycle the petroleum substance in oily sludge, thereby realize the innoxious of oily sludge and recycling target.
Accompanying drawing explanation
Fig. 1 is the experiment flow sketch of disposal of oily sludge.
Fig. 2 is the Temperature Programmed Processes sketch of disposal of oily sludge.
Embodiment
Embodiment 1:
The volume of microwave heating reactor of the present invention is 3000ml, and configuration microwave power 10KW, adopts computer program to control Heating temperature and heat-up rate.Laboratory sample is the dewatered sludge of oily water treatment, and water ratio is 79.32% (mass ratio), oil length 13.53% (mass ratio).Specific experiment step and experimental result are as follows: consult Fig. 1 and Fig. 2.
The first step, dress sample.With sample box, take laboratory sample 1000g, inserted in microwave heating reactor, then to reactor, carry out airtight.
Second step, drying and other treatment.Under the strict airtight condition of reactor, start heating system, control 60 ℃/min of temperature rise rates, make the temperature in reactor be increased to 250 ℃ by room temperature, and constant temperature is to till no longer including cut and overflowing.The result that its cut carries out condensation separation and metering is: without non-condensable gas and recovery oil mass, the recovery water yield is 795g substantially.
The 3rd step, pyrolysis processing.Continue heating, control 80 ℃/min of temperature rise rates, make reactor temperature be increased to 700 ℃, petroleum component and other organic matter in oily sludge are distilled and thermo-cracking under high temperature action, and constant temperature is to till no longer including cut and overflowing.The result that its cut carries out condensation separation and metering is: non-condensable gas 21g, refiltered oil 113g, substantially without reclaiming the water yield.In non-condensable gas, C1～C3 hydrocarbon component approaches 90%, and wherein methane content is about 50%; In refiltered oil, the light component content such as gasoline, kerosene and diesel oil is higher, roughly in 60% left and right.
The 4th step, calcination is processed.Control 100 ℃/min of temperature rise rates, make reactor temperature continue to be increased to 900 ℃, and thermostatically heating 1 minute, make the thorough coking of pyrolysis residue, then close heating system, finish experiment, the heat residue that burns takes out after naturally cooling 24hr.This process is overflowed without cut substantially, and the bright residue of heat is weighed as 253g, and oleaginousness does not detect.
Claims (1)
1. the heat treated experimental technique of oily sludge, is characterized in that:
Oily sludge sample is inserted in microwave heating reactor, adopt temperature-programmed mode to carry out heat treated to oily sludge, to the metering of product generation and to product composition analysis; Microwave heating reactor volume is 2000～3000mL; The oily sludge sample amount of inserting is 1000～2000g; Its Temperature Programmed Processes is:
The first step, drying and other treatment: oily sludge sample is elevated to 200～250 ℃ from room temperature, it is 60 ℃/min that drying and other treatment is controlled temperature rise rate, moisture is evaporated completely, complete the drying and other treatment of oily sludge, its cut carries out condensation separation, measures respectively the generation of non-condensable gas, refiltered oil and recycle-water, analyzes non-condensable gas and reclaims oil composition;
Second step, pyrolysis processing: again the oily sludge temperature after drying and other treatment is elevated to 600～700 ℃, it is 80 ℃/min that pyrolysis processing is controlled temperature rise rate, make heavy oil in oily sludge, bituminous matter organic substance carry out complete cracking under heating, complete pyrolysis processing, its cut carries out condensation separation, measures respectively the generation of non-condensable gas, refiltered oil and recycle-water, analyzes the composition of refiltered oil and non-condensable gas;
The 3rd step, calcination is processed: oily sludge pyrolysis residue temperature is elevated to 800～900 ℃, calcination processing controls temperature rise rate is 100 ℃/min, make the complete coking of pyrolysis residue, completing calcination processes, the bright residue of heat takes out and weighs after being cooled to room temperature, analyzes the content of petroleum-type pollutent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210078373.1A CN102849905B (en) | 2012-03-22 | 2012-03-22 | Experimental method of oil-containing sludge heat treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210078373.1A CN102849905B (en) | 2012-03-22 | 2012-03-22 | Experimental method of oil-containing sludge heat treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102849905A CN102849905A (en) | 2013-01-02 |
| CN102849905B true CN102849905B (en) | 2014-01-15 |
Family
ID=47396955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210078373.1A Active CN102849905B (en) | 2012-03-22 | 2012-03-22 | Experimental method of oil-containing sludge heat treatment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102849905B (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923670B (en) * | 2014-04-17 | 2016-04-20 | 杰瑞能源服务有限公司 | The industrial processing method of oil field waste and device thereof |
| CN105414155A (en) * | 2015-12-28 | 2016-03-23 | 北京中石大能源技术服务有限公司 | Harmless treatment method and harmless treatment device for industrial petroleum wastes |
| CN107200452B (en) * | 2016-03-18 | 2020-11-13 | 中国石油化工股份有限公司 | Device and method for microwave pyrolysis of sludge |
| CN107304096A (en) * | 2016-04-21 | 2017-10-31 | 李润超 | A kind of oily sludge pyrolysis processing technology |
| CN108238706B (en) * | 2016-12-23 | 2024-03-15 | 上海金匙环保科技股份有限公司 | System and process for step-by-step pyrolysis treatment of oily sludge |
| CN108786726A (en) * | 2018-05-24 | 2018-11-13 | 北京科技大学 | A kind of method that tank bottom oil sludge prepares carbon material adsorbing material |
| CN108706849A (en) * | 2018-05-28 | 2018-10-26 | 中国科学院城市环境研究所 | A kind of oily sludge classification pyrolysis plant and method |
| CN108675589A (en) * | 2018-07-23 | 2018-10-19 | 哈尔滨金源伟业环保科技有限公司 | A kind of continous way greasy filth pyrolysis treatment systems and pyrolysis treating method |
| CN108911456B (en) * | 2018-08-07 | 2021-11-05 | 李明泽 | Novel oily sludge treatment method and system |
| CN109293190B (en) * | 2018-11-02 | 2020-07-24 | 南华大学 | Treatment method of oily sludge |
| CN111377579B (en) * | 2018-12-29 | 2022-02-08 | 中国石油化工股份有限公司 | Oil sludge treatment method |
| CN109678307A (en) * | 2019-02-21 | 2019-04-26 | 阮文渊 | A kind of Three-section type heating non-stick pan oily sludge pyrolysis installation |
| CN110590087B (en) * | 2019-07-24 | 2022-07-01 | 中国石油大学(华东) | Treatment method of oily sludge |
| CN112898787A (en) * | 2021-01-25 | 2021-06-04 | 重庆交通大学 | Sludge biological asphalt and preparation method thereof |
| CN115180789A (en) * | 2022-07-08 | 2022-10-14 | 深圳市城市公共安全技术研究院有限公司 | Sludge treatment method, sludge treatment apparatus, and storage medium |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005230704A (en) * | 2004-02-19 | 2005-09-02 | Nippon Steel Corp | Method for treating oil-containing sludge |
| CN100513337C (en) * | 2006-07-28 | 2009-07-15 | 中国石油天然气股份有限公司 | Resource treating method for oil-containing sludge |
-
2012
- 2012-03-22 CN CN201210078373.1A patent/CN102849905B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102849905A (en) | 2013-01-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102849905B (en) | Experimental method of oil-containing sludge heat treatment | |
| Zhang et al. | Microwave-assisted pyrolysis of biomass for bio-oil production | |
| Lam et al. | Microwave-heated pyrolysis of waste automotive engine oil: Influence of operation parameters on the yield, composition, and fuel properties of pyrolysis oil | |
| Zuo et al. | The important role of microwave receptors in bio-fuel production by microwave-induced pyrolysis of sewage sludge | |
| Wang et al. | Experimental study of the bio-oil production from sewage sludge by supercritical conversion process | |
| Kang et al. | Fast pyrolysis of radiata pine in a bench scale plant with a fluidized bed: Influence of a char separation system and reaction conditions on the production of bio-oil | |
| Wang et al. | Hydrocarbon fuel production from soapstock through fast microwave-assisted pyrolysis using microwave absorbent | |
| Lam et al. | A review on waste to energy processes using microwave pyrolysis | |
| Islam et al. | Pyrolytic oil from fixed bed pyrolysis of municipal solid waste and its characterization | |
| Lam et al. | Microwave pyrolysis, a novel process for recycling waste automotive engine oil | |
| Kuan et al. | Catalytic pyrolysis of sugarcane bagasse by using microwave heating | |
| Wang et al. | Biomass temperature profile development and its implications under the microwave-assisted pyrolysis condition | |
| Chen | Microwave pyrolysis of oily sludge with activated carbon | |
| Li et al. | Investigation on the co-pyrolysis of agricultural waste and high-density polyethylene using TG-FTIR and artificial neural network modelling | |
| Cheng et al. | Evaluation of oil sludge ash as a solid heat carrier in the pyrolysis process of oil sludge for oil production | |
| Ibrahim | Introductory chapter: pyrolysis | |
| Ma et al. | Study on the characteristics of microwave pyrolysis of high-ash sludge, including the products, yields, and energy recovery efficiencies | |
| Zhou et al. | The effects of pyrolytic conditions on microwave pyrolysis of prairie cordgrass and kinetics | |
| Li et al. | Microwave pyrolysis of sludge: a review | |
| Zaafouri et al. | Enhancement of biofuels production by means of co-pyrolysis of Posidonia oceanica (L.) and frying oil wastes: Experimental study and process modeling | |
| Liang et al. | Effects of microwave pretreatment on catalytic fast pyrolysis of pine sawdust | |
| CN107200452B (en) | Device and method for microwave pyrolysis of sludge | |
| Al-Salem | Valorisation of end of life tyres (ELTs) in a newly developed pyrolysis fixed-bed batch process | |
| Chia Yang et al. | CONTROLLED MICROWAVE-INDUCED PYROLYSIS OF WASTE RUBBER TIRES. | |
| Cascarosa et al. | Pyrolysis of meat-meal and bone-meal blends in a mechanically fluidized reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 100007 Dongcheng District, Dongzhimen, China, North Street, No. 9 Oil Mansion, No. Co-patentee after: Beijing Aisuo in energy saving and Environmental Protection Technology Co. Ltd. Patentee after: China Petroleum & Natural Gas Co., Ltd. Address before: 100007 Dongcheng District, Dongzhimen, China, North Street, No. 9 Oil Mansion, No. Co-patentee before: Beijing National Petroleum Aisuo Environment Engineering Technology Co., Ltd. Patentee before: China Petroleum & Natural Gas Co., Ltd. |
|
| CP01 | Change in the name or title of a patent holder |