CN102849905A - Experimental method of oil-containing sludge heat treatment - Google Patents
Experimental method of oil-containing sludge heat treatment Download PDFInfo
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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 the 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 that produces in oil production and the 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 the oil refining scale, the quantity that oily sludge produces is more and more, and is more and more serious to harm, the pollution of environment.Therefore, carry out from the oily sludge refiltered oil, realize the research of residue harmlessness disposing, the environment challenge that the energy shortage problem that solves Chinese national economy sustainable development process is faced is significant.
At present, oily sludge recycling treatment technology can be divided into: physical chemistry transformation technology and thermal transition technology.Wherein, the material chemical treatment method such as extracting process, hot water wash method, is only applicable to oleaginousness at the oily sludge more than 5～10%, and needs to add chemical agent, still has sewage, waste sludge discharge, and processing costs is higher.The thermal transition technology, such as burning disposal with make fuel, brickmaking technology, although can process thoroughly the harmful poisonous organism in the oily sludge, but need set up incinerator, add simultaneously combustion-supporting fuel, exhaust gas emission is arranged, can not reclaim the crude oil in the oily sludge, exhaust gas emission is arranged, also easily secondary pollution.In all multi-methods, pyrolytic technique not only is conducive to improve the oil recovery rate of oily sludge, but and under comparatively high temps the coking of part heavy bitumen material become solid carbon, solidify in the oily sludge objectionable impuritiess such as heavy metal, realize the innoxious of pyrolysis residue.Therefore, the research of oily sludge pyrolytic technique more and more is 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 is different from traditional heating mode as a kind of emerging technology, and it is the body heating that material is caused by dielectric loss at elect magnetic field, and its energy transmits with the 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 and material had selectivity, have the characteristics such as katalysis.Although the report that adopts microwave-heating technical finesse oily sludge is arranged, its main purpose is as sorbing material the modification of the process of the residue after the oily sludge pyrolysis.Microwave have wavelength short (1～1mm) frequency high (300～300GHZ), the obvious characteristic such as Quantum Properties.People are applied to stationery, timber, the physical refining process such as resin extruded with 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 the horizontal rotation gas retort and is carried out pyrolysis processing, pyrolysis processing was reacted 1～5 hour under 200～600 ℃ of conditions, refiltered oil air water cut and pyrolysis residue.It is characterized in that the 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, and this will cause, and the treatment facility scale is large, investment is high, and 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, under 200～900 ℃ of temperature, carry out pyrolysis processing, the oil gas water that pyrolysis processing is produced carries out recycling, residue after the pyrolysis is made roadbed material or is utilized nitric acid or utilize NaOH alkali to carry out modification, and the residue after the modification is done sorbing material.The method remains the net result of only having considered that the temperature range that can carry out pyrolysis and product reclaim, and can't 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: provide reliable, the efficient easily oily sludge of science innoxious experimental technique with resource utilization for the oily sludge Pollution abatement of petroleum and petrochemical industry provides a kind of, the support that provides the scientific research basic methods for environment protection and the cleaner production of oil field refinery production process.
The inventive method is achieved in that the heat treated experimental technique of oily sludge is that the oily sludge sample is inserted in the microwave heating reactor, adopt temperature-programmed mode that oily sludge is carried out heat treated, by generation and the compositional analysis to heat-treated products, with the research heat treated feature of oily sludge and effect.Its Temperature Programmed Processes is:
The first step, drying and other treatment.The oily sludge sample is elevated to 200～250 ℃ from room temperature, moisture is evaporated fully, finish 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 that the organic substance such as heavy oil, bituminous matter carries out complete cracking because of high-temperature heating in the greasy filth, finish 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.
In the 3rd step, calcination is processed.Oily sludge pyrolysis residue temperature is elevated to 800～900 ℃, makes the complete coking of pyrolysis residue, finish the calcination of pyrolysis residue and process, the bright residue of heat takes out after being cooled to room temperature weighs, and analyzes the content of the pollutents such as petroleum-type.
The 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.
Drying and other treatment control temperature rise rate is 10～60 ℃/minute, and top temperature is 200～250 ℃.
Pyrolysis processing control temperature rise rate is 50～80 ℃/minute, 600～700 ℃ of top temperatures.
Calcination processing controls temperature rise rate is 70～100 ℃/minute, 800～900 ℃ of top temperatures.
Drying and other treatment, pyrolysis processing and calcination are processed the high temperature cut that produces and are carried out independent condensation separation, respectively non-condensable gas, refiltered oil and recycle-water are measured, respectively to the detection of taking a sample of non-condensable gas and refiltered oil.
Beneficial effect of the present invention: the present invention utilizes microwave heating technique, moisture according to the oily sludge height, form complicated characteristics, adopt the temperature programming mould that sample is carried out heat treated, by to generation and compositional analysis at the heat-treated products of different heating section, can effectively understand moisture and the heated volatile of oil component and the situation of decomposition in the 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 that the oily sludge of oil field Petrochemical Enterprises is processed, not only can reduce oily sludge to the pollution of environment, and be conducive to recycle the petroleum substance in the oily sludge, thus the innoxious and recycling target of realization oily sludge.
Description of drawings
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 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).Concrete experimental procedure and experimental result are as follows: consult Fig. 1 and Fig. 2.
The first step, the dress sample.Take by weighing laboratory sample 1000g with sample box, it is inserted in the microwave heating reactor, then carry out airtight to reactor.
Second step, drying and other treatment.Under the strict airtight condition of reactor, start heating system, 60 ℃/minute of control temperature rise rates make the temperature in the reactor be increased to 250 ℃ by room temperature, and constant temperature is till no longer include cut and overflow.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, 80 ℃/minute of control temperature rise rates make reactor temperature be increased to 700 ℃, and petroleum component and other organic matter in the oily sludge are distilled and thermo-cracking under high temperature action, and constant temperature is till no longer include cut and overflow.The result that its cut carries out condensation separation and metering is: non-condensable gas 21g, refiltered oil 113g is substantially without reclaiming the water yield.C1 in the non-condensable gas～the C3 hydrocarbon component is near 90%, and wherein methane content is about 50%; The light component content such as gasoline, kerosene and diesel oil are higher in the refiltered oil, roughly about 60%.
In the 4th step, calcination is processed.100 ℃/minute of temperature rise rates of control 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, and the heat residue that burns takes out behind 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 (7)
1. heat treated experimental technique of oily sludge is characterized in that:
The oily sludge sample is inserted in the microwave heating reactor, adopt temperature-programmed mode that oily sludge is carried out heat treated and the metering of product generation and compositional analysis; Its Temperature Programmed Processes is:
The first step, drying and other treatment: the oily sludge sample is elevated to 200～250 ℃ from room temperature, moisture is evaporated fully, finish 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 the greasy filth organic substance such as heavy oil, bituminous matter under heating, carry out complete cracking, finish 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;
In the 3rd step, calcination is processed: oily sludge pyrolysis residue temperature is elevated to 800～900 ℃, makes the complete coking of pyrolysis residue, finish the calcination of pyrolysis residue and process, the bright residue of heat takes out after being cooled to room temperature weighs, and analyzes the content of the pollutents such as petroleum-type.
2. the heat treated experimental technique of a kind of oily sludge according to claim 1, it is characterized in that: the microwave heating reactor volume is 1000～5000ml, the best is 2000～3000ml.
3. the heat treated experimental technique of a kind of oily sludge according to claim 1, it is characterized in that: the sample amount of inserting of Pyrolysis Experiment is 1000～3000g, the best is 1000～2000g.
4. the heat treated experimental technique of a kind of oily sludge according to claim 1 is characterized in that: drying and other treatment control temperature rise rate is 10～60 ℃/minute, and top temperature is 200～250 ℃.
5. the method for innocent treatment of a kind of oily sludge according to claim 1 is characterized in that: pyrolysis processing control temperature rise rate is 50～80 ℃/minute, 600～700 ℃ of top temperatures.
6. the method for innocent treatment of a kind of oily sludge according to claim 1, it is characterized in that: calcination processing controls temperature rise rate is 70～100 ℃/minute, 800～900 ℃ of top temperatures.
7. the method for innocent treatment of a kind of oily sludge according to claim 1, it is characterized in that: drying and other treatment, pyrolysis processing and calcination are processed the high temperature cut that produces and are carried out independent condensation separation, respectively non-condensable gas, refiltered oil and recycle-water are measured, respectively to the detection of taking a sample of non-condensable gas and refiltered oil.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923670A (en) * | 2014-04-17 | 2014-07-16 | 杰瑞能源服务有限公司 | Industrial treatment method and industrial treatment device for oil field waste |
| 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 |
| CN107200452A (en) * | 2016-03-18 | 2017-09-26 | 中国石油化工股份有限公司 | The device and method of microwave-heating sludge |
| CN107304096A (en) * | 2016-04-21 | 2017-10-31 | 李润超 | A kind of oily sludge pyrolysis processing technology |
| CN108238706A (en) * | 2016-12-23 | 2018-07-03 | 上海金匙环保科技股份有限公司 | Oily sludge substep pyrolysis treatment systems and technique |
| 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 |
| 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 |
| 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 |
| CN108911456A (en) * | 2018-08-07 | 2018-11-30 | 李明泽 | A kind of new process for treating oil-containing sludge and system |
| CN109293190A (en) * | 2018-11-02 | 2019-02-01 | 南华大学 | A kind of processing method of oily sludge |
| 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 |
| CN110590087A (en) * | 2019-07-24 | 2019-12-20 | 中国石油大学(华东) | Treatment method of oily sludge |
| CN111377579A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Oil sludge treatment method |
| CN113214668A (en) * | 2021-01-25 | 2021-08-06 | 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 |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103923670A (en) * | 2014-04-17 | 2014-07-16 | 杰瑞能源服务有限公司 | Industrial treatment method and industrial treatment device for oil field waste |
| 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 |
| CN107200452A (en) * | 2016-03-18 | 2017-09-26 | 中国石油化工股份有限公司 | The device and method of microwave-heating sludge |
| 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 |
| CN108238706A (en) * | 2016-12-23 | 2018-07-03 | 上海金匙环保科技股份有限公司 | Oily sludge substep pyrolysis treatment systems and technique |
| 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 |
| CN108911456A (en) * | 2018-08-07 | 2018-11-30 | 李明泽 | A kind of new process for treating oil-containing sludge and system |
| CN108911456B (en) * | 2018-08-07 | 2021-11-05 | 李明泽 | Novel oily sludge treatment method and system |
| CN109293190A (en) * | 2018-11-02 | 2019-02-01 | 南华大学 | A kind of processing method of oily sludge |
| CN111377579A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Oil sludge treatment method |
| 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 |
| CN110590087A (en) * | 2019-07-24 | 2019-12-20 | 中国石油大学(华东) | Treatment method of oily sludge |
| CN113214668A (en) * | 2021-01-25 | 2021-08-06 | 重庆交通大学 | Sludge biological asphalt and preparation method thereof |
| CN113214668B (en) * | 2021-01-25 | 2022-08-23 | 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 |
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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. |