CN106746485A - A kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment - Google Patents
A kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment Download PDFInfo
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- CN106746485A CN106746485A CN201611193261.5A CN201611193261A CN106746485A CN 106746485 A CN106746485 A CN 106746485A CN 201611193261 A CN201611193261 A CN 201611193261A CN 106746485 A CN106746485 A CN 106746485A
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- oily sludge
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/18—Treatment of sludge; Devices therefor by thermal conditioning
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/06—Treatment of sludge; Devices therefor by oxidation
- C02F11/08—Wet air oxidation
- C02F11/086—Wet air oxidation in the supercritical state
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Treatment Of Sludge (AREA)
Abstract
The present invention is a kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment, and SCWO technologies are applied to the harmless treatment of steel rolling oily sludge and recycling by the special nature that the method has using water under SCWO states.Under specific pressure, temperature, time and peroxide multiple, water and sludge infinitely dissolve, fast reaction, steel rolling oily sludge decrement more than 99.68%, and water outlet COD is down to COD and reaches 78 ~ 80mg/L by 25031mg/L, during produce micro-molecular gas reclaimed and utilized.The volume of remaining solid product is only 1.5% or so of oily sludge volume, remaining solid product is mainly made up of inorganic particulate matter, wherein Fe elements are mainly maghemite, bloodstone in the existence form of solid slag phase, are respectively provided with certain resource recycling value.Illustrate that using SCWO methods treatment steel rolling oily sludge minimizing, innoxious and recycling can be realized.
Description
Technical field
Iron and steel enterprise's steel rolling oily sludge is directed to the invention belongs to resource, field of Environment Protection, more particularly to one kind, is faced using super
Boundary's water oxidation technology (SCWO) treatment carries out the SCWO technology steel rolling oily sludge decrement harmless treatments of decrement harmless treatment
Method.
Background technology
At present, sludge disposal technology mainly has landfill, biology, burning method etc..Landfill method is to ambient contamination；Bioanalysis
The treatment oil content sludge cycle higher is more long, and clearance is than relatively low；Burning method treatment oily sludge be also easy to produce secondary pollution and
Subsequent treatment is complicated.SCWO technologies are widely used in terms of municipal sludge treatment, but are not yet related in steel rolling sludge.
The content of the invention
In order to solve the above problems, a kind of process cycle of present invention offer is short, clearance SCWO technology steel rolling higher
Oily sludge decrement method for innocent treatment.
The technical scheme is that：A kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment, the program
Specifically include following steps：
First, a certain amount of undiluted steel rolling oily sludge is put into stirred autoclave inside and fixed reactor top cover,
Temperature controller, the power switch of heater are opened, then the water in waste water cup is squeezed into reaction by double plunger high-pressure pump by preheater
Kettle, water and sludge are heated to temperature to 400-440 DEG C in reactor, and double plunger high-pressure pump starts the dioxygen in dioxygen cup
Water injects stirred autoclave, is 23-25MPa, peroxide multiple 100-300% in pressure, and the reaction time is 1-5min, and reaction terminates
Afterwards, the liquid in the outflow of gas-liquid separator delivery port is collected and determines water outlet COD value, and the recovery of gas is carried out in gaseous phase outlet,
Remaining solid product is obtained to be reclaimed and material phase analysis.
Further, the gas includes carbon dioxide, vapor, nitrogen.
Further, the volume of the remaining solid product is only less than the 1.5% of oily sludge volume, mud decrement
More than 98.5% remaining solid product is mainly made up of inorganic particulate matter, and wherein Fe elements are main in the existence form of solid slag phase
It is maghemite, bloodstone.
Further, the water outlet COD is down to 78~80mg/L by 25031mg/L.
The present invention is using (temperature and pressure of water are increased to T=374.3 DEG C of critical point, p=under supercriticality
More than 22.05MPa) the unexistent special nature of water：It can uniformly mix with air, oxygen and some organic matters, if super
Simultaneously dissolved with oxygen and organic matter in critical, then organic matter can rapidly be oxidized to small point of carbon dioxide, vapor, nitrogen etc.
Sub- compound.Achievement in research：It was found that under specific pressure, temperature, time and peroxide multiple, steel rolling oily sludge decrement
98.5% or so, and water outlet COD is very small compared with the COD numerical value that before processing is up to 25031mg/L, reaction terminates rear water outlet
COD reaches 78~80mg/L, and clarity and running water are as good as, and organic matter is substantially thoroughly decomposed in oily sludge, therefore SCWO
It is innoxious that technology can in a short time make steel rolling oily sludge reach decrement.During produce micro-molecular gas reclaimed
And utilization.The volume of remaining solid product is only 1.5% or so of oily sludge volume, and remaining solid product is main by inorganic particulate
Grain thing composition, wherein Fe elements are mainly maghemite, bloodstone in the existence form of solid slag phase, are respectively provided with certain resource
Recycle value.SCWO technologies are applied to the harmless treatment of steel rolling oily sludge and recycling, are the engineering
Using offer scientific basis and reference.
The beneficial effects of the invention are as follows：Due to using above-mentioned technical proposal, steel rolling oily sludge decrement after the method treatment
98.5% or so, and water outlet COD is very small compared with the COD numerical value that before processing is up to 25031mg/L, reaction terminates rear water outlet
COD reaches 78~80mg/L or so, and clarity and running water are as good as, therefore SCWO technologies can realize that steel rolling contains in a short time
Greasy dirt harmless treatment.During produce micro-molecular gas reclaimed and utilized.The volume of remaining solid product is only
1.5% or so of oily sludge volume, remaining solid product is mainly made up of inorganic particulate matter, and wherein Fe elements are in solid slag phase
Existence form be mainly maghemite, bloodstone, be respectively provided with certain resource recycling value.Illustrate using at SCWO methods
Reason steel rolling oily sludge can realize minimizing and recycling.
Brief description of the drawings
Fig. 1 is to scheme through the SEM that supercritical water oxidation is processed without sludge.
Fig. 2 is to scheme through the SEM that supercritical water oxidation is processed through sludge.
Fig. 3 is the XRD of residual solid after being processed through supercritical water oxidation.
Fig. 4 is the steel rolling oily sludge COD value anaplasia at any time under 440 DEG C of temperature, pressure 25MPa, peroxide multiple 300%
Change curve synoptic diagram.
Fig. 5 is the weightless figure of sludge differential thermal analysis.
Specific embodiment
Technical scheme is described further with reference to specific embodiment.
Embodiment 1：
Undiluted steel rolling oily sludge is put into stirred autoclave inside and reactor top cover is fixed, opening temperature controller,
The power switch of heater, then double plunger high-pressure pump waste water cup in water reactor, water and sludge are squeezed into by preheater
Temperature to 400 DEG C is heated in reactor, double plunger high-pressure pump starts the hydrogen peroxide in dioxygen cup to inject stirring reaction
Kettle, is 23MPa in pressure, and peroxide multiple 150%, the reaction time is 1min, after reaction terminates, in gas-liquid separator delivery port stream
The liquid for going out is collected and determines water outlet COD value, and the recovery of gas is carried out in gaseous phase outlet, is obtained remaining solid product and is reclaimed
And material phase analysis.
Embodiment 2：
Undiluted steel rolling oily sludge is put into stirred autoclave inside and reactor top cover is fixed, opening temperature controller,
The power switch of heater, then double plunger high-pressure pump waste water cup in water reactor, water and sludge are squeezed into by preheater
Temperature to 420 DEG C is heated in reactor, double plunger high-pressure pump starts the hydrogen peroxide in dioxygen cup to inject stirring reaction
Kettle, is 24MPa in pressure, and peroxide multiple 100%, the reaction time is 2min, after reaction terminates, in gas-liquid separator delivery port stream
The liquid for going out is collected and determines water outlet COD value, and the recovery of gas is carried out in gaseous phase outlet, is obtained remaining solid product and is reclaimed
And material phase analysis.
Embodiment 3：
Undiluted steel rolling oily sludge is put into stirred autoclave inside and reactor top cover is fixed, opening temperature controller,
The power switch of heater, then double plunger high-pressure pump waste water cup in water reactor, water and sludge are squeezed into by preheater
Temperature to 440 DEG C is heated in reactor, double plunger high-pressure pump starts the hydrogen peroxide in dioxygen cup to inject stirring reaction
Kettle, is 25MPa in pressure, and peroxide multiple 300%, the reaction time is 5min, after reaction terminates, in gas-liquid separator delivery port stream
The liquid for going out is collected and determines water outlet COD value, and clearance respectively reaches 97.88%, and the recovery of gas is carried out in gaseous phase outlet, is obtained
Reclaimed to remaining solid product and material phase analysis.
Embodiment 4：
Undiluted steel rolling oily sludge is put into stirred autoclave inside and reactor top cover is fixed, opening temperature controller,
The power switch of heater, then double plunger high-pressure pump waste water cup in water reactor, water and sludge are squeezed into by preheater
Temperature to 430 DEG C is heated in reactor, double plunger high-pressure pump starts the hydrogen peroxide in dioxygen cup to inject stirring reaction
Kettle, is 25MPa in pressure, and peroxide multiple 180%, the reaction time is 3.5min, after reaction terminates, in gas-liquid separator delivery port
The liquid of outflow is collected and determines water outlet COD value, and clearance respectively reaches 97.88%, and the recovery of gas is carried out in gaseous phase outlet,
Remaining solid product is obtained to be reclaimed and material phase analysis
Embodiment 5：
Undiluted steel rolling oily sludge is put into stirred autoclave inside and reactor top cover is fixed, opening temperature controller,
The power switch of heater, then double plunger high-pressure pump waste water cup in water reactor, water and sludge are squeezed into by preheater
Temperature to 410 DEG C is heated in reactor, double plunger high-pressure pump starts the hydrogen peroxide in dioxygen cup to inject stirring reaction
Kettle, is 23MPa in pressure, and peroxide multiple 200%, the reaction time is 4min, after reaction terminates, in gas-liquid separator delivery port stream
The liquid for going out is collected and determines water outlet COD value, and clearance respectively reaches 97.88%, and the recovery of gas is carried out in gaseous phase outlet, is obtained
Reclaimed to remaining solid product and material phase analysis
As Figure 1-Figure 2：Fig. 1 is the SEM figures of sludge before reaction, and Fig. 2 is the SEM figures of reacted sludge；Before processing
The surface of oily sludge is presented cotton-shaped, relatively more sticky；Remaining solid is substantially loose little particle after treatment, and size is less than 25
μm, mainly silt and metallic salt, they do not flow out with reaction solution, have reached the effect of good separation and stable metal ion
Really, the removal effect of organic matter is obvious.Water outlet is as clear as crystal, and stench disappears, and realizes harmless treatment.Using overcritical water oxygen
Changing technical finesse steel rolling oily sludge can not only realize harmless treatment, and effect is also highly significant in terms of mud decrement.
The volume of remaining solid product is only 1.5% or so of oily sludge volume, has reached the purpose of minimizing, with landfill and system fertilizer
Compare, pathogenic microorganism present in sludge, parasite and stench niff disappear, also produced in the absence of in burning process
Bioxin noxious materials.It is high through the remaining solid iron content after SCWO technical finesses, such as in Fig. 3, remaining solid mainly by by
Maghemite, calcium sulfate, silica, bloodstone, water phosphorus hydrogen sodium stone and zincblende etc. are constituted, and wherein Fe elements are in solid slag phase
Existence form be mainly maghemite, bloodstone, have recycling potentiality, can further purify and realize the utilization of resources.Always
The advantages of not only reacting fast, simple to operate, environmentally friendly using SCWO methods treatment steel rolling oily sludge, and reached and subtracted
Quantization, the innoxious and utilization of resources.
Solid residual components after treatment are analyzed as follows:
Table residual solid constituent
| Composition | Fe2O3 | SO3 | SiO2 | Na2O | CaO | ZnO | Al2O3 | P2O5 | MgO |
| Content (%) | 33.23 | 22.87 | 13.52 | 9.44 | 7.76 | 4.37 | 3.44 | 1.81 | 1.14 |
Iron-holder is high, has recycling to be worth.
Claims (3)
1. a kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment, it is characterised in that the program specifically include with
Lower step：
First, a certain amount of undiluted steel rolling oily sludge is put into stirred autoclave inside and fixed reactor top cover, is opened
The power switch of temperature controller, heater, then double plunger high-pressure pump waste water cup in water reactor, water are squeezed into by preheater
Temperature to 400-440 DEG C is heated in reactor with sludge, double plunger high-pressure pump starts the hydrogen peroxide note in dioxygen cup
Enter stirred autoclave, be forced into pressure for 23-25MPa, peroxide multiple 100-300%, the reaction time is 1-5min, and reaction terminates
Afterwards, the liquid in the outflow of gas-liquid separator delivery port is collected and determines water outlet COD value, and the recovery of gas is carried out in gaseous phase outlet,
Remaining solid product is obtained to be reclaimed and material phase analysis.
2. method according to claim 1, it is characterised in that the volume of the remaining solid product is only that oily sludge holds
Long-pending less than 1.5%, the remaining solid product of mud decrement more than 98.5% is mainly made up of inorganic particulate matter, and wherein Fe elements are solid
The existence form of body slag phase is mainly maghemite, bloodstone.
3. method according to claim 1, it is characterised in that the water outlet COD is down to 78 ~ 80mg/L by 25031mg/L.
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| CN201611193261.5A CN106746485A (en) | 2016-12-21 | 2016-12-21 | A kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment |
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| CN201611193261.5A CN106746485A (en) | 2016-12-21 | 2016-12-21 | A kind of SCWO technologies steel rolling oily sludge decrement method for innocent treatment |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006021069A (en) * | 2004-07-06 | 2006-01-26 | Toyo Koatsu Co Ltd | Reaction apparatus using supercritical water |
| CN101066828A (en) * | 2007-06-12 | 2007-11-07 | 大庆石油学院 | Technological process of treating oil-containing sludge with supercritical water oxidation |
| US20080073292A1 (en) * | 2004-11-15 | 2008-03-27 | Chematur Engineering Ab | Reactor and Method for Supercritical Water Oxidation |
| CN102503066A (en) * | 2011-12-23 | 2012-06-20 | 南京工业大学 | System and method for supercritical water oxidation treatment and resource utilization of organic sludge |
| CN103936201B (en) * | 2014-04-30 | 2015-12-02 | 贵州省环境科学研究设计院 | Fenton method associating supercritical water oxidation method treating refuse percolate |
-
2016
- 2016-12-21 CN CN201611193261.5A patent/CN106746485A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006021069A (en) * | 2004-07-06 | 2006-01-26 | Toyo Koatsu Co Ltd | Reaction apparatus using supercritical water |
| US20080073292A1 (en) * | 2004-11-15 | 2008-03-27 | Chematur Engineering Ab | Reactor and Method for Supercritical Water Oxidation |
| CN101066828A (en) * | 2007-06-12 | 2007-11-07 | 大庆石油学院 | Technological process of treating oil-containing sludge with supercritical water oxidation |
| CN102503066A (en) * | 2011-12-23 | 2012-06-20 | 南京工业大学 | System and method for supercritical water oxidation treatment and resource utilization of organic sludge |
| CN103936201B (en) * | 2014-04-30 | 2015-12-02 | 贵州省环境科学研究设计院 | Fenton method associating supercritical water oxidation method treating refuse percolate |
Non-Patent Citations (2)
| Title |
|---|
| BAOCHENCUI ETAL.: ""Oxidation of oily sludge in supercritical water"", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
| DAOAN ZOU ETAL.: ""Supercritical water oxidation of tannery sludge: Stabilization of chromium and destruction of organics"", 《CHEMOSPHERE》 * |
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