CN108408956A - The method for activating persulfate oxidation degradation of dye waste water based on persistent free radicals - Google Patents
The method for activating persulfate oxidation degradation of dye waste water based on persistent free radicals Download PDFInfo
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- CN108408956A CN108408956A CN201810103962.8A CN201810103962A CN108408956A CN 108408956 A CN108408956 A CN 108408956A CN 201810103962 A CN201810103962 A CN 201810103962A CN 108408956 A CN108408956 A CN 108408956A
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- waste water
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- water based
- oxidation degradation
- persistent free
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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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)
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The present invention provides a kind of methods activating persulfate oxidation degradation of dye waste water based on persistent free radicals, and biological sludge is air-dried, biological sludge particle is ground into；It takes biological sludge particle to be put into stainless steel cauldron, deionized water, sealing is added, then magnetic agitation is heated and reacted；After reaction, cooling, cleaning, vacuum filter, obtain sludge base activated coke；It takes sludge base activated coke to be dispersed in waste water from dyestuff, adjusts pH value to 6.8 7.6, persulfate, room temperature oscillation is then added；It is separated by solid-liquid separation after reaction, supernatant is stood, and then measures absorbance and total content of organic carbon.Present invention process process is simple, secondary pollution is small, percent of decolourization is high, it is at low cost, low energy consumption, using sludge base activated coke surface persistent free radicals activation persulfate generate with strong oxidizing property potentiometric titrations, hydroxyl radical free radical and singlet oxygen, can fast degradation dye molecule, have wide engineering application prospect.
Description
Technical field
The invention belongs to industrial wastewater treatment technology fields, more particularly to a kind of to activate persulfuric acid based on persistent free radicals
The method of salt oxidative degradation waste water from dyestuff.
Background technology
Waste water from dyestuff have high water big, coloration and organic concentration, water quality and pH value variation greatly, complicated component etc. it is special
In addition point also contains residual dye, slurry, auxiliary agent, fiber impurity and inorganic salts etc., belongs to the poor industry of biochemical in waste water
Waste water.At this stage, shortage of water resources and pollutant emission have become the conditionality factor of dyeing sustainable development.In order to
Meet the increasingly strict discharge standard of waste water from dyestuff and comprehensive recycling standard, conventional waste water treatment process must carry out upgrading and change
It makes, and combined depth treatment process, further to remove the pollutant that secondary biochemical treatment technique cannot remove, such as dissolubility
Hardly degraded organic substance etc..
Although currently, being achieved using some such as photochemistry, electrochemistry and advanced oxidation even depth processing waste water from dyestuff
Good result, but due to the restriction of the factors such as processing cost, energy consumption and secondary pollution, these technical matters are not yet useless in dyestuff
It is widely popularized in water depth processing.In addition, in order to seek efficiently to remove recalcitrant substance and nitrogen phosphorus in waste water from dyestuff
The technical method of equal nutriments, domestic and international correlation scholar and engineer also develop some new technologies and new process in succession, such as
Free-radical oxidation technology etc., it includes thermal activation, ferrous salt work that persulfate activation method, which generates potentiometric titrations mainly, at present
Change, benzoquinones activation etc., but using the research of persistent free radicals activation persulfate generation potentiometric titrations, and applied to work
The report of industry Sewage advanced treatment is considerably less.
Invention content
The technical problem to be solved by the present invention is to how remove the difficult for biological degradation object in waste water from dyestuff efficiently at low cost
Matter.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is to provide one kind was activated based on persistent free radicals
The method of oxide sulfate degradation of dye waste water, which is characterized in that step is：
Step 1：Biological sludge is air-dried, biological sludge particle is ground into；Biological sludge particle is taken to be put into stainless steel
In reaction kettle, deionized water, sealing is added, magnetic agitation is reacted after heating；After reaction, cooling, cleaning, vacuum filter,
Obtain sludge base activated coke；
Step 2：It takes the sludge base activated coke that step 1 prepares gained to be dispersed in waste water from dyestuff, adjusts pH value to 6.8-
7.6, persulfate, room temperature oscillation is then added；Be separated by solid-liquid separation after reaction, supernatant stand, then measure absorbance and
Total content of organic carbon.
Preferably, in the step 1, a diameter of 2-4mm of biological sludge particle, stainless steel cauldron volume is 100mL.
Preferably, in the step 1, the mass ratio of biological sludge and deionized water is 0.05-0.20.
Preferably, in the step 1, magnetic agitation speed 600-800r/min.
Preferably, in the step 1,1-4h is reacted after being heated to 200-260 DEG C.
Preferably, in the step 1, cleaning includes three steps：Hydrochloric acid flushing, ethyl alcohol or acetone soak, deionized water
It rinses, wherein concentration of hydrochloric acid 0.1-0.5mol/L, ethyl alcohol or acetone volume fraction are 50%-85%.
Preferably, in the step 2, waste water from dyestuff is reactive dye or azo dye wastewater, and coloration is 800-1200 times,
Organic carbon concentration is 10-15mg/L.
Preferably, in the step 2, sludge base activated coke and persulfate mass ratio are 1.0-5.0.
Preferably, in the step 2, persulfate is sodium peroxydisulfate or potassium peroxydisulfate.
Preferably, in the step 2, frequency of oscillation 100-300r/min, duration of oscillation 30-90min；Supernatant is quiet
Set to 0 .5-2h.
Compared with prior art, the present invention has the advantages that：
(1) the method for the present invention technical process is simple, and secondary pollution is small, and percent of decolourization is high, at low cost, overcomes the advanced oxygen of tradition
Chemical industry skill equipment requirement and the high defect of processing cost, can be engineered and be applied in waste water from dyestuff advanced treating.
(2) present invention utilizes special physico-chemical property and solvation effect of the distilled water under subcritical state, realizes to life
The carbonization of object sludge and aromatization process, can not only loss-rate conventional pyrolytic process it is low, and its surface endurance free love base abundance
Height, can strengthen activation persulfate generate with strong oxidizing property potentiometric titrations, and cooperate with generate hydroxyl radical free radical and
Singlet oxygen, being capable of efficient oxidation degradation of dye molecule.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.
Embodiment 1
Biological sludge is air-dried, the particle of 2mm is ground into, 5g is taken to be put into the stainless steel cauldron that volume is 100mL
In, 20mL deionized waters, sealing is added, control magnetic agitation speed is 600r/min, is then heated to 200 DEG C of reaction 1h, instead
After answering, by reaction kettle cooled to room temperature, the solidliquid mixture of reaction gained is poured out in beaker, uses 20mL concentration
It is rinsed for 0.1mol/L hydrochloric acid, then the ethyl alcohol for being 85% with 20mL volume fractions impregnates, and is then rinsed using 40mL deionizations, very
Sky filtering, obtains 2.6g sludge base activated cokes after finally weighing.
The sludge base activated coke for weighing the above-mentioned gained of 20mg is dispersed in reactive blue dye waste water, and chroma in waste water is 800 times,
Organic carbon concentration is 10mg/L, adjusts pH value to 6.8, is then rapidly added 40mg sodium peroxydisulfates, and room temperature vibrates 30min, control
Frequency of oscillation processed is 100r/min, is separated by solid-liquid separation after reaction, and supernatant stands 0.5h.After measured, decoloring dye waste water rate
It is 90%, total organic Carbon removal 71%.
Embodiment 2
Biological sludge is air-dried, the particle of 4mm is ground into, 5g is taken to be put into the stainless steel cauldron that volume is 100mL
In, 10mL deionized waters, sealing is added, control magnetic agitation speed is 800r/min, is then heated to 260 DEG C of reaction 4h, instead
After answering, by reaction kettle cooled to room temperature, the solidliquid mixture of reaction gained is poured out in beaker, uses 10mL concentration
It rinses, then the acetone soak for being 50% with 10mL volume fractions, is then rinsed using 20mL deionizations, very for 0.1mol/L hydrochloric acid
Sky filtering, obtains 2.0g sludge base activated cokes after finally weighing.
The sludge base activated coke for weighing the above-mentioned gained of 50mg is dispersed in acid red dye waste water, and coloration is 1200 times, always
A concentration of 15mg/L of organic carbon adjusts pH value to 7.6, is then rapidly added 150mg sodium peroxydisulfates, and room temperature vibrates 90min, control
Frequency of oscillation is 300r/min, is separated by solid-liquid separation after reaction, and supernatant stands 2h.After measured, decoloring dye waste water rate is
98%, total organic Carbon removal 83%.
The above, only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, can also make
Several improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution of any equivalent variations made by above-described embodiment, still fall within the range of technical scheme of the present invention
It is interior.
Claims (10)
1. a kind of method activating persulfate oxidation degradation of dye waste water based on persistent free radicals, which is characterized in that step
For：
Step 1：Biological sludge is air-dried, biological sludge particle is ground into；Biological sludge particle is taken to be put into stainless steel reaction
In kettle, deionized water, sealing is added, magnetic agitation is reacted after heating；After reaction, cooling, cleaning, vacuum filter, obtain
Sludge base activated coke；
Step 2：It takes the sludge base activated coke that step 1 prepares gained to be dispersed in waste water from dyestuff, adjusts pH value to 6.8-7.6, so
After be added persulfate, room temperature oscillation；It is separated by solid-liquid separation after reaction, supernatant is stood, and then measures absorbance and total organic
Carbon content.
2. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 1, a diameter of 2-4mm of biological sludge particle, stainless steel cauldron volume is 100mL.
3. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 1, the mass ratio of biological sludge and deionized water is 0.05-0.20.
4. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 1, magnetic agitation speed 600-800r/min.
5. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 1,1-4h is reacted after being heated to 200-260 DEG C.
6. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 1, cleaning includes three steps：Hydrochloric acid rinses, ethyl alcohol or acetone soak, deionized water rush
It washes, wherein concentration of hydrochloric acid 0.1-0.5mol/L, ethyl alcohol or acetone volume fraction are 50%-85%.
7. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 2, waste water from dyestuff is reactive dye or azo dye wastewater, and coloration is 800-1200 times,
Organic carbon concentration is 10-15mg/L.
8. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 2, sludge base activated coke and persulfate mass ratio are 1.0~5.0.
9. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 2, persulfate is sodium peroxydisulfate or potassium peroxydisulfate.
10. a kind of side activating persulfate oxidation degradation of dye waste water based on persistent free radicals as described in claim 1
Method, it is characterised in that：In the step 2, frequency of oscillation 100-300r/min, duration of oscillation 30-90min；Supernatant is quiet
Set to 0 .5-2h.
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| CN201810103962.8A CN108408956A (en) | 2018-02-01 | 2018-02-01 | The method for activating persulfate oxidation degradation of dye waste water based on persistent free radicals |
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| CN201810103962.8A CN108408956A (en) | 2018-02-01 | 2018-02-01 | The method for activating persulfate oxidation degradation of dye waste water based on persistent free radicals |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110861A (en) * | 2018-09-18 | 2019-01-01 | 中山大学 | A kind of application of municipal sludge in the treatment of waste water |
| CN110282719A (en) * | 2019-07-16 | 2019-09-27 | 东华大学 | A method of based on sludge base activated coke activated hydrogen peroxide oxidative degradation waste water from dyestuff |
| CN110282691A (en) * | 2019-07-16 | 2019-09-27 | 东华大学 | A method of based on I2 doping sludge base activated coke photocatalytic degradation of dye waste water |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110861A (en) * | 2018-09-18 | 2019-01-01 | 中山大学 | A kind of application of municipal sludge in the treatment of waste water |
| CN110282719A (en) * | 2019-07-16 | 2019-09-27 | 东华大学 | A method of based on sludge base activated coke activated hydrogen peroxide oxidative degradation waste water from dyestuff |
| CN110282691A (en) * | 2019-07-16 | 2019-09-27 | 东华大学 | A method of based on I2 doping sludge base activated coke photocatalytic degradation of dye waste water |
| CN110282691B (en) * | 2019-07-16 | 2021-10-26 | 东华大学 | Method for photocatalytic degradation of dye wastewater based on iodine-doped sludge-based activated coke |
| CN110282719B (en) * | 2019-07-16 | 2021-12-10 | 东华大学 | Method for degrading dye wastewater based on sludge-based activated coke activated hydrogen peroxide oxidation |
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