CN109704539A - A kind of recycling treatment method of oil-bearing sludge - Google Patents
A kind of recycling treatment method of oil-bearing sludge Download PDFInfo
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Abstract
The present invention relates to technical field of sludge treatment, disclose a kind of recycling treatment method of oil-bearing sludge, the method first carries out deoiling treatment to oily sludge, charing process is carried out after obtained de-oiling sludge is mixed with bio-waste again, the method carries out deoiling treatment to oily sludge in advance, and energy consumption needed for both having reduced charing process improves the pyrolysis efficiency of sludge, the quality of carbonization product is optimized again, while can also sufficiently recycle crude oil；The a certain amount of biomass castoff with a large amount of holes is added during sludge carbonization not only contributes to pyrolyzing sludge reaction and petroleum vapor recovery, and improve the quality of sludge carbon, so that final sludge carbon not only contains good structure feature, but also contain certain nutrient, further widen its application range.
Description
Technical field
The present invention relates to technical field of sludge treatment, and in particular to a kind of recycling treatment method of oil-bearing sludge.
Background technique
Oily sludge is a kind of dangerous solid waste of generation during oil field development, oil storage and transportation and oil product refining etc.
Object has been put into " National Hazard waste register " HW08 class danger containing poisonous and harmful substances such as a large amount of polycyclic aromatic hydrocarbon, heavy metals
Dangerous waste, domestic annual oily sludge generates total amount and is up to 5,000,000 tons, and yield is in increased trend year by year, these oil-containings
It just fills or stacks on the spot if sludge is unprocessed, serious adverse effect can be generated to surrounding enviroment.Therefore, containing sludge
Harmless treatment has become petrochemical industry, one of urgent problem to be solved in environmental protection.
Currently, the processing of oily sludge mainly has bioanalysis, pyrogenic process, heat treating process etc., wherein heat treating process has place
It manages thoroughly, the features such as energy recovery rate is high, and reduced training is good, it is effective to become one kind containing sewage sludge harmlessness, energy processing
Method.If Chinese patent literature CN106957136A discloses a kind of processing method containing sludge, this method is by oily sludge
Heating stirring is separated by solid-liquid separation after standing, obtains greasy filth and oily liq；Oily liq is passed through sewage disposal system to carry out
The oil of separation is carried out purification by liquid extraction by water-oil separating；It is quenched that medicament progress is added into greasy filth, it is de- to carry out depth after quenched again
Water obtains dewatered greasy filth and filtrate, and filtrate is carried out to the operation of water-oil separating again；Dewatered greasy filth is carried out at desiccation
Reason, pyrolysis carbonization treatment.However, the ingredient due to different regions oily sludge is different, imitated to reach preferable de-oiling
Fruit, this method needs the corresponding medicament kind of reselection after analyzing sludge components, and is selected according to different medicament kinds
Dosage, heating temperature, centrifugal rotational speed and centrifugation time of medicament etc. operate comparatively laborious, higher cost, are not suitable for pushing away on a large scale
Wide application.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is that process for treating oil-containing sludge in the prior art is overcome to need
Corresponding medicament kind of reselection etc. leads to cumbersome, higher cost defect after analysis sludge components, to provide one kind
Recycling treatment method of oil-bearing sludge.
In order to solve the above technical problems, the present invention provides a kind of recycling treatment method of oil-bearing sludge, including following step
It is rapid:
(1) it by oily sludge heating stirring, stands, separation obtains greasy filth and oily liq；
(2) water, wood vinegar and demulsifier are added in Xiang Suoshu greasy filth, heating stirring is stood, and separation obtains de-oiling sludge
And oily liq；
(3) biomass castoff and the de-oiling sludge are sufficiently mixed, obtain mixed material, the biomass castoff
Mass ratio with de-oiling sludge is 1:(3~5)；
(4) mixed material is subjected to charing process in 550~650 DEG C, inert gas environment.
Further, in step (2), the mass ratio of the greasy filth and the water is 1:(8~10), the matter of the wood vinegar
Amount is the 20~30% of greasy filth quality, and the quality of demulsifier is the 5~15% of greasy filth quality.
Further, in step (3), the biomass castoff is one of agricultural crop straw, timber, bamboo wood or several
Kind.
Further, before the step (3) further include: be dehydrated the de-oiling sludge to its water content≤30%
The step of.
Further, before the step (4) further include: carry out the step of being granulated processing to the mixed material.
Further, the step (4) further include: gas solid separation is carried out to the product of the charing process, obtains sludge
The step of charcoal solid and flue gas.
Further, the step (4) further include: the flue gas is condensed, obtain imflammable gas, tar and
The step of wood vinegar.
Further, the step (4) further include: the tar and the wood vinegar are separated, by isolated wood
Vinegar liquid is used for the step of step (2).
Further, the step (4) further include: burn the imflammable gas, the spoke that will be generated in combustion process
Heat is penetrated for thermal energy needed for providing step (1), step (2), at least one in step (4).
Further, further includes: step (1) and step (2) oily liq are subjected to water-oil separating, it will be isolated
Oil carry out purification by liquid extraction, the step of isolated water is used for the step (2).
Technical solution of the present invention has the advantages that
1. recycling treatment method of oil-bearing sludge provided by the invention, the method first carries out at de-oiling oily sludge
Reason, then carries out charing process after obtained de-oiling sludge is mixed with bio-waste, the method in advance to oily sludge into
Row deoiling treatment, energy consumption needed for both having reduced charing process improves the pyrolysis efficiency of sludge, and optimizes the product of carbonization product
Matter, while can also sufficiently recycle crude oil；It is discarded that a certain amount of biomass with a large amount of holes is added during sludge carbonization
Object not only contributes to pyrolyzing sludge reaction and petroleum vapor recovery, and improves the quality of sludge carbon, so that final sludge carbon is not
Only contain good structure feature, but also contain certain nutrient, further widens its application range.
2. recycling treatment method of oil-bearing sludge provided by the invention, the method further limits greasy filth and water and wood
The dosage of vinegar liquid improves the oil removal rate of oily sludge.
3. recycling treatment method of oil-bearing sludge provided by the invention, the method also includes taking off to de-oiling sludge
Water, water takes away a large amount of heat when effectively preventing because of pyrolysis, improves the pyrolysis efficiency of sludge, and avoids water oil after cooling mixed
It closes, causes Water-In-Oil and oil-in-water problem to occur, reduce the expense of back segment water-oil separating and sewage treatment；In addition, sludge is pre-
After dehydration, hot flue gas is directly contacted with sludge, and heat-transfer effect is good, and the thermal efficiency is high, substantially reduces the cost of pyrolysis system；Again
Person, after sludge pre-dehydration, viscosity is increased, more fully mixed with stalk, improves the uniformity of granulation, improves dirt
The quality of peat.
4. recycling treatment method of oil-bearing sludge provided by the invention, to the mixed material of sludge and biomass castoff into
Row granulation processing, increases the density of the mixed material, reduces the gap between material, reduces the air that material carries, and improves
The efficiency of sludge anaerobic charing.
5. recycling treatment method of oil-bearing sludge provided by the invention, the method has effectively achieved mud, oil, water three-phase
Separation, and it is each mutually can be recycled after separation, the utilization rate of resource is greatly improved, reduces production cost, and solve
The problem of offal treatment.Relative to traditional treatment method, the processing method provided by the present invention not only can solve existing sludge
Problem of environmental pollution caused by method of disposal, and can also sufficiently recycle the organic matter lain in sludge and N P and K etc.
Soil nutrient elements.
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
Embodiment 1
Present embodiments provide a kind of recycling treatment method of oil-bearing sludge, comprising the following steps:
(1) by oily sludge heating stirring, heating temperature is 60 DEG C, speed of agitator 30r/min, is consolidated after standing 1h
Liquid separation, obtains greasy filth and oily liq；
(2) water, wood vinegar and demulsifier NaCl are added into the greasy filth of step (1), wherein the matter of the quality of water and greasy filth
For amount than being 1:9, the quality that the quality of wood vinegar is 25%, NaCl of greasy filth quality is the 10% of greasy filth quality, heating stirring, is added
Hot temperature is 80 DEG C, speed of agitator 30r/min, is separated by solid-liquid separation after standing 1h, obtains de-oiling sludge and oily liq；
(3) the de-oiling sludge in step (2) is subjected to by way of extruding mechanical dehydration and obtains water content≤60%
Just dehydration de-oiling sludge；First dehydration de-oiling sludge heating, drying is obtained into the dehydration de-oiling sludge of water content≤30% again；
(4) biomass castoff and the dehydration de-oiling sludge of step (3) are sufficiently mixed with 1:4 (w/w), obtain mixture
Material；
(5) mixed material of step (4) is sent into pelletizer, extrusion granulation, obtaining length is 2~4cm, and diameter is
The elongated particle of 1cm；
(6) mixed material after granulation is sent into retort, in 600 DEG C, N2Charing 2h is carried out under conditions of protection, is obtained
To sludge carbon and hot fume；
Cooling hot fume, obtains imflammable gas, wood vinegar and tar in such a way that three-level condensing tower sprays wood vinegar；
Burn combustible gas is used to provide the radiant heat generated in combustion process to step (1), step (2) and step
(6) thermal energy needed for；Isolated wood vinegar is used for step (2) and purification hot fume；
(7) oily liq in step (1) and step (2) is subjected to water-oil separating, isolated oil is extracted
Reuse is purified, isolated water is used for step (2).
Embodiment 2
Present embodiments provide a kind of recycling treatment method of oil-bearing sludge, comprising the following steps:
(1) by oily sludge heating stirring, heating temperature is 70 DEG C, speed of agitator 30r/min, is consolidated after standing 1h
Liquid separation, obtains greasy filth and oily liq；
(2) water, wood vinegar and demulsifier CaCl are added into the greasy filth of step (1)2, the wherein matter of the quality of water and greasy filth
For amount than being 1:8, the quality of wood vinegar is 20%, CaCl of greasy filth quality2Quality be greasy filth quality 15%, heating stirring,
Heating temperature is 70 DEG C, speed of agitator 30r/min, is separated by solid-liquid separation after standing 1.5h, obtains de-oiling sludge and containing oil liquid
Body；
(3) the de-oiling sludge in step (2) is subjected to by way of extruding mechanical dehydration and obtains water content≤60%
Just dehydration de-oiling sludge；First dehydration de-oiling sludge heating, drying is obtained into the dehydration de-oiling sludge of water content≤20% again；
(4) biomass castoff and the dehydration de-oiling sludge of step (3) are sufficiently mixed with 1:3 (w/w), obtain mixture
Material；
(5) mixed material of step (4) is sent into pelletizer, extrusion granulation, obtaining length is 2~4cm, and diameter is
The elongated particle of 1cm；
(6) mixed material after granulation is sent into retort, in 550 DEG C, N2Charing 3h is carried out under conditions of protection, is obtained
To sludge carbon and hot fume；
Cooling hot fume, obtains imflammable gas, wood vinegar and tar in such a way that three-level condensing tower sprays wood vinegar；
Burn combustible gas, thermal energy needed for being used to provide the radiant heat generated in combustion process to step (6)；It will be isolated
Wood vinegar is for step (2) and purification hot fume；
(7) oily liq in step (1) and step (2) is subjected to water-oil separating, isolated oil is extracted
Reuse is purified, isolated water is used for step (2).
Embodiment 3
Present embodiments provide a kind of recycling treatment method of oil-bearing sludge, comprising the following steps:
(1) by oily sludge heating stirring, heating temperature is 50 DEG C, speed of agitator 30r/min, is carried out after standing 1.5h
It is separated by solid-liquid separation, obtains greasy filth and oily liq；
(2) water, wood vinegar and demulsifier ferric trichloride and polyaluminium sulfate are added into the greasy filth of step (1), wherein water
Quality and the mass ratio of greasy filth be 1:10, the quality of wood vinegar is the 30% of greasy filth quality, ferric trichloride and polyaluminium sulfate
Quality be respectively the 2.5% of greasy filth quality, heating stirring, heating temperature be 90 DEG C, speed of agitator 30r/min, stand 1h
After be separated by solid-liquid separation, obtain de-oiling sludge and oily liq；
(3) the de-oiling sludge in step (2) is subjected to by way of extruding mechanical dehydration and obtains water content≤60%
Just dehydration de-oiling sludge；First dehydration de-oiling sludge heating, drying is obtained into the dehydration de-oiling sludge of water content≤20% again；
(4) biomass castoff and the dehydration de-oiling sludge of step (3) are sufficiently mixed with 1:5 (w/w), obtain mixture
Material；
(5) mixed material of step (4) is sent into pelletizer, extrusion granulation, obtaining length is 2~4cm, and diameter is
The elongated particle of 1cm；
(6) mixed material after granulation is sent into retort, in 650 DEG C, N2Charing 3h is carried out under conditions of protection, is obtained
To sludge carbon and hot fume；
Cooling hot fume, obtains imflammable gas, wood vinegar and tar in such a way that three-level condensing tower sprays wood vinegar；
Burn combustible gas is used to provide the radiant heat generated in combustion process to step (1), step (2) and step
(6) thermal energy needed for；Isolated wood vinegar is used for step (2) and purification hot fume；
(7) oily liq in step (1) and step (2) is subjected to water-oil separating, isolated oil is extracted
Reuse is purified, isolated water is used for step (2).
Comparative example 1
This comparative example provides a kind of process for treating oil-containing sludge, operates according to Chinese patent literature CN106957136A
Middle embodiment 1.
Comparative example 2
This comparative example provides a kind of process for treating oil-containing sludge, and substantially with embodiment 1, difference exists specific steps
In that wood vinegar is not added in step (2), but the aluminium polychloride and 0.5% of oily sludge absolute dry weight 0.5% being added
Sodium peroxydisulfate.
The measurement of 1 oil removal rate of experimental example
Oil removal rate measurement, measuring method are carried out to the pretreated de-oiling sludge of 1-3 of the embodiment of the present invention and comparative example 1-2
It is as follows with measurement result.
Measuring method:
The untreated oily sludge of 10g is weighed, is packed with qualitative filter paper, Soxhlet extraction device extraction is then placed in, uses
Filtrate filtering is quantitatively arrived 100mL, using the oil-containing of determined by ultraviolet spectrophotometry oily sludge by 80mL petroleum ether reflux 3.5h
Measure w1；Pretreated 10g de-oiling sludge is weighed respectively, petroleum ether is added, is extracted with Soxhlet extraction device, is returned with 80mL petroleum ether
3.5h is flowed, 100mL is quantitatively arrived into filtrate filtering, using the resid amount w of determined by ultraviolet spectrophotometry de-oiling sludge2；According to
Lower formula calculates, and obtains corresponding oil removal rate.Oil removal rate calculation formula is as follows:
Measurement result is shown in Table 1:
The oil removal rate of 1 distinct methods of table
| Test | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 |
| Oil removal rate (%) | 92.1 | 90.5 | 91.3 | 64.4 | 64.7 |
Method of the invention is used it can be seen from the data in upper table 1, the oil removal rate of oily sludge is high, and what is obtained is de-
Greasy dirt resid amount is low.
2 different material biomass carbon specific surface of experimental example and pore-size distribution
The sludge carbon of the embodiment of the present invention 1 and specific surface area of other types of biomass carbon, total pore volume, total is measured respectively
Micro pore volume and mean pore sizes, wherein biomass carbon specific area, pore-size distribution are using V-Sorb 2800P specific surface and aperture point
Analyzer (Beijing Jin Ai science popularization Co., Ltd) measurement, measurement result are shown in Table 2:
2 different material biomass carbon specific surface of table and pore-size distribution
It, can by the data in upper table 2 it is found that adopting the sludge carbon being obtained by the present invention has good pore structure
It is used as soil conditioner.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of recycling treatment method of oil-bearing sludge, which comprises the following steps:
(1) it by oily sludge heating stirring, stands, separation obtains greasy filth and oily liq；
(2) water, wood vinegar and demulsifier are added in Xiang Suoshu greasy filth, heating stirring is stood, and separation obtains de-oiling sludge and contains
Oil liquid body；
(3) biomass castoff and the de-oiling sludge are sufficiently mixed, obtain mixed material, the biomass castoff and de-
The mass ratio of greasy dirt is 1:(3~5)；
(4) mixed material is subjected to charing process in 550~650 DEG C, inert gas environment.
2. the method according to claim 1, wherein in step (2), the mass ratio of the greasy filth and the water is
1:(8~10), the quality of the wood vinegar is the 20~30% of greasy filth quality, the quality of demulsifier be greasy filth quality 5~
15%.
3. method according to claim 1 or 2, which is characterized in that in step (3), the biomass castoff is farming
One or more of object stalk, timber, bamboo wood.
4. method according to claim 1-3, which is characterized in that before the step (3) further include: to described
The step of de-oiling sludge is dehydrated to its water content≤30%.
5. method according to claim 1-4, which is characterized in that before the step (4) further include: to described
Mixed material carries out the step of being granulated processing.
6. method according to claim 1-5, which is characterized in that the step (4) further include: to the charing
The step of product of processing carries out gas solid separation, obtains sludge carbon solid and flue gas.
7. according to the method described in claim 6, it is characterized in that, the step (4) further include: carried out to the flue gas cold
The step of coagulating, obtaining imflammable gas, tar and wood vinegar.
8. the method according to the description of claim 7 is characterized in that the step (4) further include: separate the tar with it is described
Wood vinegar, the step of isolated wood vinegar is used for the step (2).
9. method according to claim 7 or 8, which is characterized in that the step (4) further include: the combustibility of burning
The radiant heat generated in combustion process is used to provide needed for step (1), step (2), at least one in step (4) by gas
Thermal energy.
10. -9 described in any item methods according to claim 1, which is characterized in that further include: by step (1) and step (2) institute
It states oily liq and carries out water-oil separating, isolated oil is subjected to purification by liquid extraction, isolated water is used for the step
(2) the step of.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110240369A (en) * | 2019-06-06 | 2019-09-17 | 中海油天津化工研究设计院有限公司 | A kind of pyrolysis of polymer-containing oil sludge-extraction cycle recycling treatment process method |
| CN110330198A (en) * | 2019-07-09 | 2019-10-15 | 北京和荣工程技术有限公司 | A kind of oil-sludge treatment method and system |
| CN114517104A (en) * | 2020-11-19 | 2022-05-20 | 中国石油化工股份有限公司 | Oily sludge-based biochar and preparation method and application thereof |
| CN115722188A (en) * | 2021-08-30 | 2023-03-03 | 中国石油化工股份有限公司 | Porous carbon-loaded metal oxide adsorbent and preparation method and application thereof |
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| CN102765866A (en) * | 2012-07-23 | 2012-11-07 | 扬州澄露环境工程有限公司 | Method for recycling urban sludge |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110240369A (en) * | 2019-06-06 | 2019-09-17 | 中海油天津化工研究设计院有限公司 | A kind of pyrolysis of polymer-containing oil sludge-extraction cycle recycling treatment process method |
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| CN114517104A (en) * | 2020-11-19 | 2022-05-20 | 中国石油化工股份有限公司 | Oily sludge-based biochar and preparation method and application thereof |
| CN114517104B (en) * | 2020-11-19 | 2023-09-05 | 中国石油化工股份有限公司 | Oily sludge-based biochar and preparation method and application thereof |
| CN115722188A (en) * | 2021-08-30 | 2023-03-03 | 中国石油化工股份有限公司 | Porous carbon-loaded metal oxide adsorbent and preparation method and application thereof |
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Application publication date: 20190503 |