CN109867421A - A kind of chromium-bearing sludge processing method and system based on supercritical water oxidation - Google Patents
A kind of chromium-bearing sludge processing method and system based on supercritical water oxidation Download PDFInfo
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- CN109867421A CN109867421A CN201910276294.3A CN201910276294A CN109867421A CN 109867421 A CN109867421 A CN 109867421A CN 201910276294 A CN201910276294 A CN 201910276294A CN 109867421 A CN109867421 A CN 109867421A
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Abstract
The chromium-bearing sludge processing method based on supercritical water oxidation that the invention discloses a kind of, by being thermally dried to sludge, after milled processed, it is diluted to the dilution sludge with certain moisture content again, after the collaboration processing of ultrasonication and supercritical water oxidation, treated, and solid liquid phase organic matter is completely degraded, Cr ion is oxidized to Cr VI and is transferred to liquid phase, solid phase residue is substantially free of heavy metal Cr, security landfill can be carried out, and the Cr in supernatant can then carry out resource utilization.Also disclose a kind of chromium-bearing sludge processing system based on supercritical water oxidation, including pretreatment unit, ultrasound processing unit and supercritical water oxidation unit；Pretreatment unit includes material storage tank, heater and grinder, and ultrasound processing unit uses processor for ultrasonic wave, and supercritical water oxidation unit includes reaction kettle, oxygen tank, temperature controller and pressure controller.
Description
Technical field
The invention belongs to field of environment protection, and in particular to a kind of chromium-bearing sludge processing based on supercritical water oxidation
Method and system.
Background technique
With the development of leather industry, leather-making mud becomes a big pollution sources of threatening environment.Leather-making mud in addition to
The major toxicity of organic pollutant is from heavy metal chromium.Chromium in leather-making mud is mainly and calcium salt mineral, crystallization iron oxygen
The compounds such as compound and crystallization chromated oxide combine, and belong to strong bound.Chromium in these reference states is in high ecological hazard wind
Danger is horizontal.Trivalent chromium in sludge can be oxidized during the reaction and be converted to Cr VI, and the toxicity of Cr VI is about three
100 times of valence chromium are strong mutation substances, there is lasting risk to environment and human body.Nowadays Cr resource reserve is not
It is abundant, belong to scarce resource, High Content Chromium is by resource utilization while being badly in need of that leather-making mud is innoxious.
Landfill and burning are the common processing disposal technologies of leather-making mud, do not carry out harmless treatment before Sludge landfill,
The sludge percolate of landfill is improper because seepage control measure, and meeting contaminated soil, surface water and underground water cause for a long time ambient enviroment
Harm.Though incineration technology has carried out minimizing processing to it, it was verified that leather-making mud complicated component, can generate a large amount of
Pernicious gas and excessive dust, especially toxic gas dioxin.In incineration residue, trivalent chromium conversion is Cr VI, toxicity
Enhancing, residue need to carry out advanced treating again.Therefore, the method for filling and burning does not solve fundamentally at three changes to sludge
Reason.
Supercritical Water Oxidation Technology, i.e. SCWO (Supercritical Water Oxidation) are developed recentlies
The novel hydrothermal oxidation technology of one kind.When water is on critical point (Tc=374.15 DEG C, Pc=22.1MPa), it is situated between
Electric constant is very low, O2、CO2It may be implemented to dissolve each other completely in supercritical water with nonpolar molecules such as organic matters, eliminate phase boundary
In face of the alternate resistance of heat and mass, CO is thoroughly converted by the hardly degraded organic substance in sludge2And H2Nitrogen is converted N by O2With
N2The innocuous substances such as O, and the elements such as phosphorus, chlorine, sulphur can be precipitated from supercritical water in the form of inorganic salts, realization is organic to be had
Noxious material it is innoxious.Supercritical technology has various advantages: 1. reaction speed is fast, and oxidation reaction is very thorough, and general
Need 10~30 seconds removal rates that can reach 99% or more.2. organic matter and oxidant can be mutual according to any ratio and supercritical water
It is molten, so that heterogeneous reaction be made to become homogeneous reaction, the pernicious gases such as SOx and NOx will not be generated and cause secondary pollution.3. organic
Object releases a large amount of heat when being oxidized, and when content of organics is greater than 3%, does not need extraneous heat supply, releases using reaction
Hot maintenance process thermal balance, realize autothermal reaction.4. it is easy to the separation of salt, in overcritical, the solubility of inorganic salts
Very low, almost all is precipitated after reaction with precipitation form.
Supercritical Water Oxidation Technology is mainly used to handle various organic polluting waters at present, utilizes supercritical water without scholar
Oxidation technology carries out some further investigations for Cr.
Summary of the invention
The purpose of the present invention is to provide a kind of chromium-bearing sludge processing method and system based on supercritical water oxidation,
It can be by the efficient resource utilization of heavy metal Cr while a large amount of harmful organic substances in removing sludge.
The present invention is to be achieved through the following technical solutions:
A kind of chromium-bearing sludge processing method based on supercritical water oxidation, comprising the following steps:
1) chromium-bearing sludge is dried, powder is made in the chromium-bearing sludge after drying process, obtains primary sludge；
2) primary sludge is diluted, obtains dilution sludge, dilution sludge is subjected to ultrasonication；
3) sludge after ultrasonication is subjected to supercritical water oxidation, the temperature of supercritical water oxidation is
470~550 DEG C, pressure is 22.1MPa or more；
4) after cooling precipitating, obtain that treated sludge and supernatant.
Further, the time of ultrasonication is 10~30min in step 2).
Further, ultrasonication uses intermittent processing in step 2).
Further, intermittent processing is specially with ultrasonic 3S, and the gap-ratio of interval 2S is handled.
Further, in step 3) when supercritical water oxidation, the intake of oxygen and the sludge after ultrasonication
COD is 1:1.
Further, supercritical water oxidation uses intermittent reaction in step 3).
The chromium-bearing sludge processing system based on supercritical water oxidation that the invention also discloses a kind of, including pretreatment are single
Member, ultrasound processing unit and supercritical water oxidation unit；
Pretreatment unit includes material storage tank, heater and grinder, and ultrasound processing unit uses processor for ultrasonic wave,
Supercritical water oxidation unit includes reaction kettle, oxygen tank, temperature controller and pressure controller；
Material storage tank, heater and grinder are sequentially connected by pipeline, and grinder passes through pipeline and processor for ultrasonic wave
Connection, processor for ultrasonic wave are connect by pipeline with reaction kettle, and oxygen tank, temperature controller, oxygen tank and temperature controller are equal
It is connect with reaction kettle.
Further, reaction kettle is also connected with cooling back installation and gas-liquid separator.
Further, reaction kettle is also connected with nitrogen gas tank.
Further, processor for ultrasonic wave is also connected with centrifuge.
Compared with prior art, the invention has the following beneficial technical effects:
The method of chromium-bearing sludge processing disclosed by the invention, is first thermally dried sludge, after milled processed, by it
It is diluted to the dilution sludge with certain moisture content, conveniently goes to measure each experimental result and performs an analysis comparison；Pass through ultrasonication
It breaks apart inorganic states salt with Cr, more Cr is made to be exposed to surface, then after being handled by supercritical water oxidation, it is solid that treated
Liquid phase organic matter is completely degraded, and Cr ionic oxide formation at Cr VI and is transferred to liquid phase, and solid phase residue is substantially free of weight
Metal Cr, considerably reduces Leaching, so that residue after reaction is become harmless substance, can carry out security landfill, and supernatant
Cr in liquid can then make mordant and carry out resource utilization.Treatment method process is simple, provides one for heavy metal sewage sludge
Kind cleans treatment process without secondary pollution.
Further, the time of ultrasonication is too short, does not have the effect for breaking apart inorganic states salt and Cr, ultrasonic treatment
Overlong time, there are the wastings of resources, have finally chosen 10~30min according to experimental study.
Further, ultrasonication uses intermittent processing, has bigger recycling effect, and be not easy at blocking
Manage device.
Further, since supercritical reaction conditions are more harsh, kettle internal corrosion can be caused in reaction process, inorganic salts are insoluble
In supercriticality, reactor may be blocked, therefore the present invention is designed as intermittent reaction, then can high degree avoid this
The generation of class problem, and intermittent reaction has bigger recycling effect.
Chromium-bearing sludge processing system disclosed by the invention based on supercritical water oxidation, including it is pretreatment unit, mixed
Close ultrasound processing unit and supercritical water oxidation unit；Pretreatment unit include sequentially connected material storage tank, heater and
Grinder, ultrasound processing unit use processor for ultrasonic wave, and supercritical water oxidation unit includes reaction kettle, oxygen tank, temperature
Controller and pressure controller.Pretreatment unit is used to carry out sludge heating grinding pretreatment, and ultrasound processing unit is used for
Sludge is ultrasonically treated, supercritical water oxidation unit for carrying out supercritical water oxidation, ultrasound processing unit and
After the collaboration processing of supercritical water oxidation unit, treated, and solid liquid phase organic matter is completely degraded, and Cr ion is oxidized to
Cr VI is simultaneously transferred to liquid phase, and solid phase residue is substantially free of heavy metal Cr, can carry out security landfill, and the Cr in supernatant is then
It can carry out resource utilization；The connection of whole system structure is compact, and construction investment is small, utilizes its overcritical technological merit, research and development
The method of pollution administration chromium mud realizes the harmless treatment to leather-making mud and the utilization of resources to heavy metal chromium, meanwhile, for
The development of its technology and engineer application is pushed to have great importance.
Further, reaction kettle is connected with cooling back installation, and supercritical water oxidation will can occur in reaction kettle in time
Heat derives, this partial heat is recycled.
Further, reaction kettle is also connected with nitrogen gas tank, purges reaction kettle with nitrogen, excludes residual air in kettle.
Further, processor for ultrasonic wave is also connected with centrifuge, ultrasound sludge separate in centrifuge later solid phase with
Liquid phase, liquid phase are used to measure the variation of supernatant SCOD, and solid phase is formed for analysis heavy metal.
Detailed description of the invention
Fig. 1 is the functional block diagram of chromium-bearing sludge processing system of the invention；
Fig. 2 is the flow chart that chromium-bearing sludge of the invention is handled；
Fig. 3 is the solid phase power spectrum front and back comparison diagram of embodiment 8, and figure (a) is the solid phase power spectrum of primary sludge as a result, figure (b)
For the solid phase power spectrum result of sludge after processing.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The process object of present system be chromium-bearing sludge, carrier include but is not limited to organic wastewater, debirs or
Sludge.
Referring to Fig. 1, a kind of chromium-bearing sludge processing system based on supercritical water oxidation of the invention, including pretreatment
Unit, ultrasound processing unit and supercritical water oxidation unit；Pretreatment unit includes material storage tank, heater and grinder,
Ultrasound processing unit use processor for ultrasonic wave, supercritical water oxidation unit include reaction kettle, oxygen tank, temperature controller and
Pressure controller；Material storage tank, heater and grinder are sequentially connected by pipeline, and grinder passes through pipeline and ultrasonication
Device connection, processor for ultrasonic wave are connect by pipeline with reaction kettle, oxygen tank, temperature controller, oxygen tank and temperature controller
It is connect with reaction kettle.
The heating method of temperature controller can be used electric heating, heat-conducting oil heating, steam heating or pass through supercritical water
Hot fluid heats after oxidation reaction.
Reaction kettle is continuous interval dual-purpose type reaction unit, but passes through experimental study, and intermittent reaction can have Cr bigger
Recycling effect, intermittent reaction is used in experiment, temperature regulating range is 0~600 DEG C, pressure regulation spectrum is 0~
40MPa need to ensure that reaction kettle does not leak pressure every time.
More preferably, reaction kettle is also connected with cooling back installation, and supercritical water oxidation will occur in reaction kettle in time
Heat derives, cooling back installation is shell-and-tube heat exchanger, and cold fluid flow flows through shell-side through pipe side, hot fluid.
More preferably, reaction kettle is also connected with gas-liquid separator, can will acquire in time the gas-phase product generated in reaction kettle,
And be discharged in atmosphere, without until being discharged again after natural cooling.
More preferably, reaction kettle is also connected with nitrogen gas tank, before entry into the trial, purges reaction kettle 3min, row with pure nitrogen gas
Except air remaining in reaction kettle, it is ensured that the accuracy of oxygenate content.
More preferably, screening machine is added between grinder and processor for ultrasonic wave, the sludge sieving after grinder is ground
Processing, obtains the sludge of uniform particle diameter.
Heater uses baking oven, and grinder uses planetary ball mill, and screening machine uses shaking-sieving instrument.
For the clearer work for illustrating the chromium-bearing sludge processing method of the invention based on supercritical water oxidation
Process, preferred embodiment given below are illustrated the specific work process of the system.
Sludge used in this experiment is aqueous after the processing such as mechanical compression after appearance from Xinji City's plum blossom tannery sludge
Rate is 70%.
Embodiment 1
A kind of method of chromium-bearing sludge processing, comprising the following steps:
1) it pre-processes: after experiment first dries this sludge for 24 hours before carrying out in 105 DEG C of high temperature ovens, guaranteeing that moisture is complete
It loses entirely.It reuses planetary ball mill to be ground into a powder solid sludges, sludge is divided into different-grain diameter using shaking-sieving instrument,
Using the sewage sludge powder under 300 meshes as primary sludge.
Weigh after taking primary sludge 1g, be put into Muffle furnace and burnt at 600 DEG C to constant weight, then after being weighed with initial value phase
Subtract to obtain the content of organic matter, the content of organic matter 49.9%.
Primary sludge 0.1000g is taken, in polytetrafluoroethylene (PTFE) crucible, the wetting of 2mL ultrapure water is added, sequentially adds
5mL98%HNO3With 2mL HF, heating (temperature is 150~200 DEG C) is done to close on electric hot plate, is removed and is cooled to room temperature.Add
Enter 5mL HF continuation heating (temperature is 150~200 DEG C) on electric hot plate to do to close.It removes and is cooled to room temperature.3~4mL is added
Nitration mixture (HNO3: HCIO4=1:1) continue heating (temperature is 110~160 DEG C) into doing, it removes and is cooled to room temperature.Use 5%HNO3
Heating for dissolving treated sample be settled to 500mL, as digestion solution, surveyed with national standard method and with 0.45 μm of membrane filtration
Obtaining total chrome content in primary sludge is 55mg/g.
Primary sludge is separated into solid phase and liquid phase in the centrifuge of 5000r/min, liquid phase is for measuring supernatant SCOD
Variation, solid phase for analysis heavy metal form.
2) supercritical water oxidation: before entry into the trial, purging reaction kettle 3min with pure nitrogen gas, excludes remaining in kettle
Air.Pretreated sludge is put into reaction kettle, sealing flange, opens temperature controller, it is set with 5 DEG C/min of temperature
Rate rise, when reaching 380 DEG C, adjustment pressure is filled with oxygen with the mistakes oxygen amount of 1:1 to 32MPa, is remembered with oxygen supply starting
Start for reaction.When end of reaction, turn off pressure and temperature, using cooling back installation natural cooling, reaction kettle is equipped with residue
Outlet and gas-liquid separator, directly obtain solid product and supernatant product, with to be measured.
Test result:
The removal rate of TOC is up to 97% in sludge, most down to 96.87mg/L.And supernatant C r is then 407.1mg/L, it is dirty
Cr in mud has 25% and is transferred to liquid phase, illustrates that also major part Cr in solid phase sludge, cannot reach recycling.
Embodiment 2
Compared with Example 1, the difference is that, the temperature of supercritical water oxidation is adjusted to 470 DEG C.
Test result:
The removal rate of TOC is up to 98.9% in sludge, most down to 16.92mg/L.And supernatant C r is then 1074.8mg/L,
Cr in sludge has 67.2% and is transferred to liquid phase, and national emission request is not achieved in sludge.
Embodiment 3
Compared with Example 1, the difference is that, the temperature of supercritical water oxidation is adjusted to 520 DEG C.
Test result:
At 520 DEG C, supernatant TOC is 15.7mg/L, and for removal rate still up to 99%, supernatant C r reaches 1219.1mg/L,
The mobility of Cr is 73.0%, and national emission request is not achieved in sludge.
Embodiment 4
Compared with Example 1, the difference is that, the temperature of supercritical water oxidation is adjusted to 550 DEG C.
Test result:
The removal rate of TOC is up to 99.45% in sludge, most down to 9.14mg/L.And supernatant C r is then 1242.9mg/L,
Cr in sludge has 78% and is transferred to liquid phase, and national emission request is not achieved in sludge.
Embodiment 5
As shown in Fig. 2, a kind of method of chromium-bearing sludge processing, comprising the following steps:
1) pre-process: after experiment first dries this sludge for 24 hours before carrying out in 105 DEG C of high temperature ovens, use is planetary
Solid sludges are ground into a powder by ball mill, and sludge is divided into different-grain diameter using shaking-sieving instrument, by the sludge powder under 300 meshes
End is used as primary sludge.
Weigh after taking primary sludge 1g, be put into Muffle furnace and burnt at 600 DEG C to constant weight, then after being weighed with initial value phase
Subtract to obtain the content of organic matter, the content of organic matter 49.9%.
Primary sludge 0.1000g is taken, in polytetrafluoroethylene (PTFE) crucible, the wetting of 2mL ultrapure water is added, sequentially adds
5mL98%HNO3With 2mL HF, (about 150~200 DEG C) are heated on electric hot plate and are done to close, removes and is cooled to room temperature.5mL is added
HF continues the heating (about 150~200 DEG C) on electric hot plate to be done to close.It removes and is cooled to room temperature.3~4mL nitration mixture (HNO is added3:
HCIO4=1:1) continue to heat (about 110~160 DEG C) into doing, it removes and is cooled to room temperature.At the heating for dissolving of 5%HNO3
Sample after reason, and with 0.45 μm of membrane filtration, it is settled to 500mL, as digestion solution, is measured in primary sludge with national standard method
Total chrome content is 55mg/g.
2) primary sludge: being diluted to the solution of 85% moisture content by ultrasonication, and 18h is shaken on shaking table to being saturated shape
State, the water for testing use is deionized water.Ultrasonic power chooses 3600W*75%, 8 φ vibration amplitude arms.Every time by 30mL muddy water
Saturation mixed liquor is put into 150mL beaker for ultrasonication, and probe is submerged beaker center 3cm depth, with ultrasonic 3S interval
The gap-ratio work 2min of 2S.
Sludge is separated solid phase and liquid phase later by ultrasound in the centrifuge of 5000r/min, and liquid phase is for measuring supernatant
The variation of SCOD, solid phase are formed for analysis heavy metal.
3) supercritical water oxidation: before entry into the trial, purging reaction kettle 3min with pure nitrogen gas, excludes remaining in kettle
Air.Sludge after ultrasonication is put into reaction kettle, sealing flange, opens temperature controller, it is set with temperature 5
DEG C/rate of min rises, and when reaching 470 DEG C, adjustment pressure to 32MPa, while oxygen is filled with the mistakes oxygen amount of 1:1, to supply oxygen
Starting is denoted as reaction and starts.When end of reaction, turn off pressure and temperature, using cooling back installation natural cooling, reaction kettle is set
There are solid discharge and gas-liquid separator, solid product and supernatant product is directly obtained, with to be measured.
Test result:
The removal rate of TOC is up to 99.06% in sludge, most down to 16.7mg/L.And the Cr in sludge has 69% transfer
To liquid phase, national emission request is not achieved in sludge.
Embodiment 6
Compared with Example 5, the difference is that, the time of ultrasonication is adjusted to 10min.
Test result:
After ultrasonic 10min, the removal rate of TOC is up to 99.25% in sludge, most down to 12.45mg/L, and the Cr in sludge
It has 85.1% and is transferred to liquid phase.
Embodiment 7
Compared with Example 5, the difference is that, the time of ultrasonication is adjusted to 20min.
Test result:
After ultrasonic 20min, TOC down to 15.1mg/L, TOC removal rate still up to the mobility of 99.5%, Cr up to 97%,
Sludge has been substantially free of Cr on to a certain degree.
Embodiment 8
Compared with Example 5, the difference is that, the time of ultrasonication is adjusted to 30min.
Test result:
1. the removal rate of TOC is up to 99.6% in sludge, most down to 6.71mg/L.Cr concentration is in supernatant
1599.5mg/L, the Cr in sludge have 99% and are transferred to liquid phase, and sludge reaches minimizing and recycling, has in the Cr of supernatant
95% with Cr6+In the presence of being more advantageous to Cr and be recycled as mordant.
2. after supersonic synergic is overcritical, solid phase Cr is from mass ratio as shown in figure 3, solid phase power spectrum result is provable
8.77% is reduced to 1.14%, and organic carbon is reduced from percentage composition 20.86% to 0.561%.The remaining Cr of solid phase is by inorganic carbon
Hydrochlorate or sulfate are wrapped in lattice, and very stable there is do not destroy it overcritical so strong condition
Structure, not only being decremented also has directly reached recycling to sludge.
Claims (10)
1. a kind of chromium-bearing sludge processing method based on supercritical water oxidation, which comprises the following steps:
1) chromium-bearing sludge is dried, powder is made in the chromium-bearing sludge after drying process, obtains primary sludge；
2) primary sludge is diluted, obtains dilution sludge, dilution sludge is subjected to ultrasonication；
3) sludge after ultrasonication being subjected to supercritical water oxidation, the temperature of supercritical water oxidation is 470~
550 DEG C, pressure is 22.1MPa or more；
4) after cooling precipitating, obtain that treated sludge and supernatant.
2. the chromium-bearing sludge processing method according to claim 1 based on supercritical water oxidation, which is characterized in that step
It is rapid 2) in ultrasonication time be 10~30min.
3. the chromium-bearing sludge processing method according to claim 1 based on supercritical water oxidation, which is characterized in that step
It is rapid 2) in ultrasonication use intermittent processing.
4. the chromium-bearing sludge processing method according to claim 3 based on supercritical water oxidation, which is characterized in that
Formula of having a rest processing is specially with ultrasonic 3S, and the gap-ratio of interval 2S is handled.
5. the chromium-bearing sludge processing method according to claim 1 based on supercritical water oxidation, which is characterized in that step
It is rapid 3) in supercritical water oxidation when, the COD of the intake of oxygen and the sludge after ultrasonication is 1:1.
6. the chromium-bearing sludge processing method according to claim 1 based on supercritical water oxidation, which is characterized in that step
It is rapid 3) in supercritical water oxidation use intermittent reaction.
7. a kind of chromium-bearing sludge processing system based on supercritical water oxidation, which is characterized in that including pretreatment unit, surpass
Sonicated unit and supercritical water oxidation unit；
Pretreatment unit includes material storage tank, heater and grinder, and ultrasound processing unit uses processor for ultrasonic wave, super to face
Boundary's water oxidation unit includes reaction kettle, oxygen tank, temperature controller and pressure controller；
Material storage tank, heater and grinder are sequentially connected by pipeline, and grinder is connect by pipeline with processor for ultrasonic wave,
Processor for ultrasonic wave is connect by pipeline with reaction kettle, oxygen tank, temperature controller, oxygen tank and temperature controller with react
Kettle connection.
8. the chromium-bearing sludge processing system according to claim 7 based on supercritical water oxidation, which is characterized in that anti-
Kettle is answered to be also connected with cooling back installation and gas-liquid separator.
9. the chromium-bearing sludge processing system according to claim 7 based on supercritical water oxidation, which is characterized in that anti-
Kettle is answered to be also connected with nitrogen gas tank.
10. the chromium-bearing sludge processing system according to claim 7 based on supercritical water oxidation, which is characterized in that
Processor for ultrasonic wave is also connected with centrifuge.
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| CN114250374A (en) * | 2022-03-01 | 2022-03-29 | 生态环境部华南环境科学研究所 | Method for efficiently extracting chromium from electroplating sludge by utilizing ultrasonic oxidation technology |
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