CN107381863A - A kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide - Google Patents
A kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide Download PDFInfo
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- CN107381863A CN107381863A CN201710607245.4A CN201710607245A CN107381863A CN 107381863 A CN107381863 A CN 107381863A CN 201710607245 A CN201710607245 A CN 201710607245A CN 107381863 A CN107381863 A CN 107381863A
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- iron oxide
- waste water
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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
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- 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
- C02F1/722—Oxidation by peroxides
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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
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic 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
- 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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The present invention relates to technical field of waste water processing, specifically discloses a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide.Methods described comprises at least following steps：First the pH value of highly salt containing organic waste water is adjusted to 4.0 6.5, ferriferous oxide catalyst is previously added, adds oxidant, Fe2+, reacted, and control pH value in course of reaction to be maintained between 4.0 6.5；Reaction is filtered after terminating, and Fe is added after filter cake plus moisture are dissipated2+, heating response is carried out, generates iron oxide red or iron oxide yellow.After preferential addition catalyst iron oxide of the invention induces reaction, Fe2+Added simultaneously with oxidant, a large amount of nano iron oxide catalysts of in-situ preparation, improve OH generation efficiencies and the degradation speed to organic matter, for TOC clearances more than 80%, degradation effect is excellent, and after the completion of degraded, grade ferric oxide product can be obtained, reaches twice laid.
Description
Technical field
The present invention relates to technical field of waste water processing, more particularly to a kind of degraded highly salt containing organic waste water and synchronously prepare oxygen
Change the method for iron.
Background technology
With developing rapidly for the industry such as China's medicine, chemical industry, oil, marine product, high saliferous organic wastewater with difficult degradation thereby row
High-volume it is being on the increase, conventional treatment method is first desalination, again biochemistry at present.For the desalination containing high-concentration organic substance wastewater,
Evaporation is most simple effective method, but conventional method of evaporating is merely capable of realizing the effect of desalination, can not be by organic contamination
Thing is degraded, and secondary pollution problems be present.Fenton and class Fenton oxidation technology due to reaction condition is gentle, equipment operation is simple,
The advantages that processing cost is quite relatively low and applied widely, and its Technical comparing is ripe, has been successfully applied to a variety of Industry Wastes
Water degradation treatment.But to still suffer from dioxygen water use efficiency low and produce a certain amount of sludge etc. and ask due to existing Fenton oxidation technology
Topic.Therefore, a kind of processing method for having organic pollution fast degradation concurrently and not producing sludge is designed to solving high salt high concentration
Organic wastewater administers problem and environmental protection has great importance.
The content of the invention
For oxidant utilization in existing high saliferous Industrial Wastewater Treatment it is low and produce sludge the problems such as, the present invention provide
A kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide.
To achieve the above object of the invention, the embodiment of the present invention employs following technical scheme：
A kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, including at least following steps：
Step 1, the pH value of highly salt containing organic waste water adjusted to 4.0-6.5, be previously added ferriferous oxide catalyst, add oxygen
Agent, Fe2+, reacted, and control pH value in course of reaction to be maintained between 4.0-6.5；
Step 2, reaction are filtered after terminating, and collect filter cake, and catalyst Fe is added after filter cake plus moisture are dissipated2+Mixed solution is obtained, will
The pH value regulation of the mixed solution carries out heating response, generates iron oxide red or iron oxide yellow between 6.5-7.
Relative to prior art, degraded highly salt containing organic waste water provided by the invention and the method for synchronously preparing iron oxide,
Have the advantage that：
（1）The present invention is previously added catalyst iron oxide, adds Fe2+, now Fe2+Can be with the three of catalyst iron oxide surface
Electronics transfer occurs for valency iron, and catalyst surface has the generation of " nascent state " ferrous iron, because the ferrous iron has extraordinary reduction
Ability, can be preferentially from H2O2Obtain being electronically generated OH, so H in theory2O2The efficiency for producing OH is 100%, is added simultaneously
The Fe entered2+Become Fe after electronics transfer3+, fast hydrolyzing in-situ preparation metastable state iron oxide yellow or iron oxide red, turn into electronics transfer again and urge
Agent.
（2）The present invention can be being realized to preparing face while high saliferous high concentrated organic wastewater oxidative degradation, desalination
Expect level iron oxide product, tinting strength, tinting power can reach more than 95%, and index meets national standard, can be used as production marketing.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, methods described
Including at least following steps：
Step 1, the pH value of highly salt containing organic waste water adjusted to 4.0-6.5, be previously added ferriferous oxide catalyst, add oxygen
Agent, Fe2+, reacted, and control pH value in course of reaction to be maintained between 4.0-6.5；
Step 2, reaction are filtered after terminating, and collect filter cake, and catalyst Fe is added after filter cake plus moisture are dissipated2+Mixed solution is obtained, will
The pH value regulation of the mixed solution carries out heating response, generates iron oxide red or iron oxide yellow between 6.5-7.
Degradation of organic waste water is mainly reacted with OH and organic matter, OH generation speed and OH and organic matter
What reaction rate determined, after preferential addition catalyst iron oxide induces reaction in the present invention, ferrous and H2O2Add simultaneously, simultaneously
The a large amount of nano iron oxide catalysts of in-situ preparation, OH generation efficiencies are improved again, and degradation rate is fast.After the completion of degraded, filter cake
After heating response, grade ferric oxide product can be obtained.
Preferably, the ferric oxide catalyst be iron oxide red, iron oxide yellow, iron oxide black, iron hydroxide, at least
One kind, addition are 0.5-2 g/L.
Preferably, oxidant described in the step 1 is H2O2、O2, air, at least one of persulfate.The step
Oxidant and Fe in rapid 12+Add simultaneously, pH value is maintained between 5.0-5.5 in course of reaction, Fe described in the step 12+
Mol ratio with oxidant is 0.8-1.2:1.
In the present invention to organic wastewater degraded mainly reacted with OH and organic matter, H2O2、O2, air or persulfuric acid
Salt can be with Fe2+Generation electronics shifts, and is quickly generated OH, oxidant can excessively cause to waste, and OH caused by very few meeting is too
Few, organic wastewater degraded is not thorough, therefore Fe2+Amount can suitably adjust, ensure by oxidant all generation OH.
The present invention is improved out-phase class Fenton's reaction, synchronous to add oxidant and Fe2+, when pH value is less than 4, it is unfavorable for
Fe3+Hydrolysis, when pH value is higher than 6.5, the Fe of addition2+Easily form Fe (OH)2, in whole course of reaction being always maintained at pH exists
5.0-5.5, substantially increases degradation efficiency, and TOC clearance can reach more than 80%.
Preferably, oxidant described in the step 1 is H2O2, addition 10-200mL/L.
H2O2Content of the addition according to organic matter in highly salt containing organic waste water.
Preferably, the Fe2+It is one kind in frerrous chloride, ferrous sulfate or iron and steel pickling waste liquid.
Fe2+Iron and steel pickling waste liquid can be selected, can twice laid, reduce cost, moreover it is possible to reach excellent degradation effect.
Preferably, in the step 3, the mass ratio of filter cake and water is 1:0.5,95-100 DEG C of heating response temperature, heating
Reaction time 2-3h.
Preferably, in the step 2, reaction is filtered after terminating, and filtrate is evaporated into moisture, leaves salt.
In the step 2, filtrate is evaporated, and moisture can be evaporated, and the COD contents after condensation is handled are low, nothing
The industrial wastewater of salinity, while the content for evaporating organic impurities in the salinity left is low, the salinity purity of recovery is higher.
Preferably, the highly salt containing organic waste water is from organic wastewater caused by biological medicine and/or fine chemistry industry.
It is provided in an embodiment of the present invention in order to better illustrate, illustrated below by embodiment is further.
Embodiment 1
The present embodiment provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, highly salt containing organic waste water choosing
From industrial wastewater caused by production DSD acid oxidation stage, wherein containing NaSO4Content is about 10wt%, total organic carbon（TOC）For
9438mg/L.Take the mL of waste water 200 to be placed in the reactor with stirring, add 0.5g iron oxide red catalyst, oxidant H2O2,
Then 30wt% H is taken respectively2O230mL and 3.7mol/L frerrous chloride 75mL, reactor is synchronously added to peristaltic pump
In, reacting liquid pH value is controlled in 5.0-5.5 with alkali lye, carries out degradation reaction, TOC is 669mg/L after degraded, and degradation efficiency is
92.9%.Water sample COD is 76 mg/L after steaming salt.Filter cake ferriferous oxide through the iron oxide red product being converted into that flows back
Color power reaches 92% (511 nm), and product pigment performance is good.
Embodiment 2
The present embodiment provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, highly salt containing organic waste water choosing
From industrial wastewater caused by production DSD acid oxidation stage, wherein containing NaSO4Content is about 10wt%, total organic carbon（TOC）For
9438mg/L.Take the mL of waste water 200 to be placed in the reactor with stirring, add 0.5g iron oxide red catalyst, oxidant is
Na2S2O8, then take respectively containing 130g Na2S2O8The aqueous solution and 3.7mol/L the mL of frerrous chloride 150, peristaltic pump is synchronous
It is added in reactor, reacting liquid pH value is controlled in 5.0-5.5 with alkali, carries out degradation reaction, and TOC is 366mg/L after degraded, drop
It is 91.3% to solve efficiency.Water sample COD is 49mg/L after steaming salt.The iron oxide that filter cake ferriferous oxide is converted into through flowing back
Red, tinting strength, tinting power reaches 97% (511 nm), and product pigment performance is good.
Embodiment 3
The present embodiment provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, highly salt containing organic waste water choosing
From industrial wastewater caused by production DSD acid oxidation stage, wherein containing NaSO4Content is about 10wt%, total organic carbon（TOC）For
9438mg/L.Take the mL of waste water 200 to be placed in the reactor with stirring, add 0.5g iron oxide red catalyst, oxidant O2,
3.7mol/L frerrous chloride 105mL is taken, is added to peristaltic pump in reactor, reacting liquid pH value is controlled in 5.0-5.5 with alkali,
Degradation reaction is carried out, TOC is 519mg/L after degraded, degradation efficiency 96%.Water sample COD is 64mg/L after steaming salt.Filter cake
The iron oxide red that ferriferous oxide is converted into through flowing back, tinting strength, tinting power reach 99% (511 nm), and product pigment performance is good.
Embodiment 4
The present embodiment provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, highly salt containing organic waste water choosing
From the industrial wastewater caused by production pesticide material medicine, wherein content containing NaCl is about 11wt%, COD 57900mg/L.Take useless
The mL of water 200 is placed in the reactor with stirring, adds 0.5g iron oxide yellow catalyst, oxidant H2O2, then take respectively
30wt% H2O2 8mL and 3.7mol/L frerrous chloride 20.6mL, synchronously it is added to peristaltic pump in reactor, course of reaction
Middle pH value is controlled in 5.0-5.5 with alkali lye.It is 10520mg/L to steam water sample COD after salt, degradation efficiency 81%.Filter cake iron
The iron oxide yellow that oxide is converted into through flowing back, tinting strength, tinting power reach 95% (511 nm), and product pigment performance is good.
Embodiment 5
The present embodiment provides a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, highly salt containing organic waste water choosing
Industrial wastewater caused by from medicine intermediate production process, wherein NaCl and ammonium chloride content are about 13wt%, protochloride
Iron is that 1.2mol/L and COD is about 11000mg/L.Take waste water 50mL to be placed in the reactor with stirring, add 0.5g iron oxide
Red catalyst, then by 200mL waste water containing ferrous salt and 30wt% H2O210mL is synchronously added in reactor, reacting liquid pH value
Controlled with alkali lye in 5.0-5.5.It is 280mg/L to steam cooling water COD after salt, degradation efficiency 98%.Filter cake ferriferous oxide
The iron oxide red being converted into through flowing back, tinting strength, tinting power reach 101% (511 nm), and product pigment performance is good.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide, it is characterised in that：Methods described is at least wrapped
Include following steps：
Step 1, the pH value of highly salt containing organic waste water adjusted to 4.0-6.5, be previously added ferriferous oxide catalyst, add oxygen
Agent, Fe2+, reacted, and control pH value in course of reaction to be maintained between 4.0-6.5；
Step 2, reaction are filtered after terminating, and collect filter cake, and catalyst Fe is added after filter cake plus moisture are dissipated2+Mixed solution is obtained, will
The pH value regulation of the mixed solution carries out heating response, generates iron oxide red or iron oxide yellow between 6.5-7.
2. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State ferric oxide catalyst for iron oxide red, iron oxide yellow, iron oxide black, iron hydroxide, at least one of, addition 0.5-
2 g/L。
3. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
It is H to state oxidant described in step 12O2、O2, air, at least one of persulfate.
4. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State oxidant and Fe in step 12+Add simultaneously, pH value is maintained between 5.0-5.5 in course of reaction.
5. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State Fe described in step 12+Mol ratio with oxidant is 0.8-1.2:1.
6. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 5, it is characterised in that：Institute
It is H to state oxidant described in step 12O2, addition 10-200mL/L.
7. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State Fe2+It is one kind in frerrous chloride, ferrous sulfate or iron and steel pickling waste liquid.
8. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State in step 3, the mass ratio of filter cake and water is 1:0.5,95-100 DEG C of heating response temperature, heating response time 2-3h.
9. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：Institute
State in step 2, reaction is filtered after terminating, and filtrate is evaporated into moisture, leaves salt.
10. degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide as claimed in claim 1, it is characterised in that：
The highly salt containing organic waste water is from organic wastewater caused by biological medicine and/or fine chemistry industry.
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| CN201710607245.4A CN107381863A (en) | 2017-07-24 | 2017-07-24 | A kind of degraded highly salt containing organic waste water and the method for synchronously preparing iron oxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083521A (en) * | 2017-12-12 | 2018-05-29 | 中海油天津化工研究设计院有限公司 | A kind of method that integrated micro oxidation reduces organic wastewater TOC |
| CN110237481A (en) * | 2018-07-10 | 2019-09-17 | 华东理工大学 | A kind of abraum salt method for innocent treatment |
| CN112875762A (en) * | 2021-01-30 | 2021-06-01 | 嘉诚环保工程有限公司 | Method for preparing iron oxide red by using iron-containing pickling waste liquid |
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| CN1033786A (en) * | 1988-11-14 | 1989-07-12 | 洪都钢厂 | Utilize iron and steel pickling waste liquid to produce the processing method of iron oxide yellow |
| US20060016762A1 (en) * | 2002-03-14 | 2006-01-26 | Cha Daniel K | Process for treating waste from the production of energetics |
| CN101559983A (en) * | 2009-05-15 | 2009-10-21 | 华南理工大学 | Method for preparing red iron oxide by utilizing materialized mud of malysite water treatment agent |
| CN104525201A (en) * | 2015-01-05 | 2015-04-22 | 华东理工大学 | Non-homogeneous-phase Fenton catalyst with magnetism and preparing method and application thereof |
| CN105712464A (en) * | 2016-04-27 | 2016-06-29 | 河北协同环保科技股份有限公司 | Fenton-like technique and reactor for treating biochemical effluent |
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2017
- 2017-07-24 CN CN201710607245.4A patent/CN107381863A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033786A (en) * | 1988-11-14 | 1989-07-12 | 洪都钢厂 | Utilize iron and steel pickling waste liquid to produce the processing method of iron oxide yellow |
| US20060016762A1 (en) * | 2002-03-14 | 2006-01-26 | Cha Daniel K | Process for treating waste from the production of energetics |
| CN101559983A (en) * | 2009-05-15 | 2009-10-21 | 华南理工大学 | Method for preparing red iron oxide by utilizing materialized mud of malysite water treatment agent |
| CN104525201A (en) * | 2015-01-05 | 2015-04-22 | 华东理工大学 | Non-homogeneous-phase Fenton catalyst with magnetism and preparing method and application thereof |
| CN105712464A (en) * | 2016-04-27 | 2016-06-29 | 河北协同环保科技股份有限公司 | Fenton-like technique and reactor for treating biochemical effluent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083521A (en) * | 2017-12-12 | 2018-05-29 | 中海油天津化工研究设计院有限公司 | A kind of method that integrated micro oxidation reduces organic wastewater TOC |
| CN110237481A (en) * | 2018-07-10 | 2019-09-17 | 华东理工大学 | A kind of abraum salt method for innocent treatment |
| CN112875762A (en) * | 2021-01-30 | 2021-06-01 | 嘉诚环保工程有限公司 | Method for preparing iron oxide red by using iron-containing pickling waste liquid |
| CN112875762B (en) * | 2021-01-30 | 2022-05-17 | 河北粤海水务集团有限公司 | Method for preparing iron oxide red by using iron-containing pickling waste liquid |
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