CN102951706B - Processing method of wastewater containing salts and chloride ions - Google Patents
Processing method of wastewater containing salts and chloride ions Download PDFInfo
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Abstract
The invention discloses a processing method of wastewater containing salts and chloride ions. According to the invention, the wastewater, a catalyst, and a catalyst protective agent are subjected to a mixing treatment under an electrochemical catalytic oxidation condition, such that B/C of processed wastewater is higher than 0.3; and the processed wastewater is subjected to solid-liquid separation. The catalyst is a metal ion catalyst. The catalyst protective agent can improve the utilization rate of the catalyst. According to the invention provided by the invention, catalyst addition amount is low, waste slag production amount is low, wastewater COD can be effectively reduced, and wastewater biodegradability is improved.
Description
Technical field
The present invention relates to the treatment process of the waste water of a kind of saliferous, chloride ion-containing.
Background technology
In industrial production and life process, often can produce the waste water of the high saliferous of a class, high chloride ion-containing, as: high saliferous dyeing waste water in high saliferous, oily(waste)water and the dye industry producing in the dense water that produces in the electric desalting waste water in refinery, industrial reverse-osmosis treated process, oil recovery process etc.Under normal circumstances, the salts contg in such waste water makes useless electrical conductivity of water up to μ s up to ten thousand, and its chloride ion content is also greater than 1000mg/L, and organism in waste water is difficult to degraded mostly.Add that because the biodegradability of such waste water itself is poor the salts contg of waste water and chloride ion content are too high, and suppress microbial growth, so be difficult to recover the oil, conventional biochemical method is processed, and adopt the treatment effect of the methods such as flocculation, filtration, film processing, distillation poor, and high cost, therefore, industrial and infeasible.Thereby for a long time, the processing of high saliferous, high chloride ion-containing waste water is one of difficult point in environmental improvement always.
Because employing electro-catalytic oxidation technology is processed high saliferous, high chloride ion-containing waste water has the advantage that treatment effect is good, treatment process is simple, with low cost and obtained research widely.As CN101723486A discloses a kind of method that adopts electrochemical catalysis method to process high saliferous, high chloride waste water, the method comprises pending saliferous, chloride ion-containing waste water is entered in electrochemical reactor, in reactor, add as-reduced metal ionic catalyst, connect the power supply on reactor negative electrode, positive electrode, make the organism generation oxidizing reaction in waste water.But the catalyst amounts of the method is many compared with generation large, waste residue, and unstable to the treatment effect of waste water.
Summary of the invention
The treatment effect that the object of the invention is to the method for wastewater treatment that overcomes prior art is unstable, and the dosage of catalyzer is large, the many defects of generation of waste residue, a kind of method that saliferous, chloride ion-containing waste water are processed that can be effectively also stable is provided, the catalyst amounts generation little, waste residue of the method is little, and can effectively reduce the COD of waste water, improve the biodegradability of waste water.
The present inventor finds, in the process that the method for the electrochemical catalytic oxidation of employing prior art is processed waste water, in reaction process, generate throw out and can not participate in again in the reaction of electrocatalysis and had a strong impact on the catalytic effect of metal ion catalyst thereby have part metals ionic catalyst, and affected the treatment effect of waste water.The present inventor, by adopt catalyst protective agent in the treating processes of waste water, forms the object of probability to reach remarkable minimizing throw out.
To achieve these goals, the invention provides the treatment process of the waste water of a kind of saliferous, chloride ion-containing, wherein, the method comprises carries out described waste water, catalyzer and catalyst protective agent combination treatment under electrochemical catalytic oxidation condition, make waste water B/C > 0.3 after treatment, then waste water after treatment is carried out to solid-liquid separation; Described catalyzer is metal ion catalyst; Described catalyst protective agent can improve the utilization ratio of catalyzer.
Method of wastewater treatment provided by the invention utilizes electrochemical catalysis principle; in the process that waste water is processed; by adopting catalyst protective agent can significantly reduce or prevent that metal ion catalyst from generating the probability of precipitation;; improve the utilization ratio of catalyzer; thereby can make full use of described catalyzer, make it to have better more stable treatment effect.And, can reduce the amount of adding catalyzer, even without adding catalyzer, thereby reduce the processing cost of waste water.Moreover the generation of waste residue is corresponding minimizing also, in meeting environmental requirement, also reduce the processing cost of waste residue.
Other features and advantages of the present invention are described in detail the embodiment part subsequently.
Embodiment
Below will be elaborated to the specific embodiment of the present invention.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
According to the present invention, the treatment process of described waste water comprises that the method comprises and described waste water, catalyzer and catalyst protective agent is carried out under electrochemical catalytic oxidation condition to combination treatment, make the B/C > 0.3 of waste water after treatment, under preferable case, the B/C that makes waste water after treatment is > 0.35; Then waste water after treatment is carried out to solid-liquid separation; Described catalyzer is metal ion catalyst; Described catalyst protective agent can improve the utilization ratio of catalyzer.
According to the present invention; as long as described waste water, catalyzer and catalyst protective agent being carried out under electrochemical catalytic oxidation condition to the method for combination treatment can guarantee under electrochemical catalytic oxidation condition; utilize catalyzer to carry out catalytic oxidation and produce free radical; and then organism in degrading waste water; reach improve waste water biodegradability (; improve the value of the B/C of waste water), the object of the COD value of reduction waste water.
Under preferable case; the method of described combination treatment comprises described waste water, catalyzer and catalyst protective agent is placed in to the electrochemical reactor with anode and negative electrode; connect the power supply of described reactor anode and negative electrode, waste water, catalyzer and catalyst protective agent are carried out under electrochemical catalytic oxidation condition to combination treatment.At the anode of described electrochemical reactor, chlorion in waste water is oxidized to chlorine, and chlorine leach generates hypochlorous acid in water, and hypochlorous acid (for example produces free radical under the effect of catalyzer, hydroxyl radical free radical), thus the organism in can degrading waste water.
According to the present invention; as long as the consumption of described electrochemical catalytic oxidation condition and catalyzer and catalyst protective agent can meet the B/C > 0.3 that makes the waste water after treatment obtaining; under preferable case; make the B/C > 0.35 of waste water after treatment; more preferably in situation, the COD value of the waste water after treatment obtaining is reached below 60mg/L.
Wherein, described electrochemical catalytic oxidation condition can be the conventional electrochemical catalytic oxidation condition of water treatment field, and for example, described electrochemical oxidation condition can comprise that strength of current is 0.1-1000A/m
2, be preferably 1-500A/m
2.
The time of described combination treatment is not particularly limited, as long as can fully make oxidation operation in waste water to improve the biodegradability of waste water, and preferably reduce the COD value of waste water, under preferable case, the time of described combination treatment can be 10-90 minute, further, under preferable case, the time of described combination treatment is 30-60 minute.
According to the present invention, in order to make the catalyzed oxidation better effects if of waste water, the pH value of described waste water is 1-7, more preferably 2-6.
According to the present invention, the anode of described electrochemical reactor and negative electrode can be anode and the negative electrode of the reactor that is applied to electrochemical catalytic oxidation reaction of this area routine, and for example, described anode can be selected from SnO
2/ Ti, PbO
2one in/Ti, Pt, graphite, active carbon fibre peacekeeping stainless steel; Be preferably SnO
2/ Ti or PbO
2/ Ti; Described negative electrode can be stainless steel electrode.
According to the present invention, described metal ion catalyst can for conventional various of water treatment field can play in catalysis waste water can catalytic specie (as chlorion) thus oxidation generate the stronger free radical of oxidisability, as the catalyzer of hydroxyl radical free radical, under preferable case, the metal in described metal ion catalyst can be selected from one or more in Fe, Mn, Ni, Co, Cd, Cu, Ag, Cr and Zn.For example, described metal ion catalyst can be one or more in vitriol, nitrate, muriate and the phosphoric acid salt etc. of above-mentioned metal.More preferably in situation, described metal ion catalyst is trivalent iron salt and/or ferrous salt.For example, can be selected from one or more in iron trichloride, ferric sulfate, iron protochloride, Iron nitrate, ferrous sulfate, iron nitrate.
Under preferable case, in metal ion in described metal ion catalyst and waste water, the mol ratio of chlorion can be 0.001-10: 1, more preferably in situation, in the metal ion in described metal ion catalyst and waste water, the mol ratio of chlorion is 0.005-5: 1.
According to the present invention, described catalyst protective agent is any catalyst protective agent that can improve the utilization ratio of catalyzer.In other words; in the treating processes of waste water; under the effect of catalyst protective agent, reduce the probability of metal ion catalyst generation oxyhydroxide; can play and reduce or prevent that described metal ion catalyst from generating sedimentary effect, and can guarantee that described metal ion catalyst fully participates in electrochemical catalytic oxidation reaction.Under preferable case, described catalyst protective agent is selected from one or more in ethylenediamine tetraacetic acid (EDTA), acetic acid, oxalic acid, citric acid and nitrilotriacetic acid(NTA).
Under preferable case, the mass ratio of described metal ion catalyst and described catalyst protective agent can be 1: 0.03-10, more preferably, in situation, the mass ratio of described metal ion catalyst and described catalyst protective agent is 1: 0.05-2.
The present inventor finds; when described catalyst protective agent is selected from any two kinds while being used in conjunction with in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), oxalic acid and citric acid; can further improve it and prevent that catalyzer from producing sedimentary effect; wherein, the mass ratio of any two kinds in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), oxalic acid and citric acid is preferably 0.1-10: 1.
According to the present invention, the method for waste water being carried out to solid-liquid separation can be the method for the various solid-liquid separation of this area routine, for example, and the methods such as gravity settling, centrifugation or filtration.Its concrete operation method and condition are conventionally known to one of skill in the art, for example, the temperature of described solid-liquid separation can be normal temperature (20-40 ℃), as long as the time of solid-liquid separation can guarantee that fully separating impurity requires with the suspended substance value that meets processed waste water, under normal circumstances, the time of solid-liquid separation can be 5-600 minute, is preferably 10-120 minute.In order to be more conducive to fully separating of solid phase and liquid phase; described waste water, metal ion catalyst and catalyst protective agent are being carried out after combination treatment under electrochemical catalytic oxidation condition; before carrying out solid-liquid separation, the pH value that regulates described waste water is 6-9, preferably 6.5-7.5.The method of described adjusting waste water ph can be the method for this area routine, for example, add acid or alkali to regulate, the concentration of acid or alkali and consumption can be adjusted according to actual needs, as long as guarantee the pH value of waste water to be adjusted to 6-9, be preferably 6.5-7.5.
According to the present invention, described waste water can be the waste water of various saliferous, chloride ion-containing, for example, high saliferous dyeing waste water in high saliferous, oily(waste)water and the dye industry producing in the dense water that produces in electric desalting waste water in refinery, industrial reverse-osmosis treated process, oil recovery process etc., under normal circumstances, B/C≤0.3 of described waste water, the COD value of waste water is generally 200-800mg/L, for more unmanageable waste water, its B/C is less than 0.1 conventionally; Described useless electrical conductivity of water is 300-200000 μ s, is preferably 500-150000 μ s; Chlorine ion concentration in described waste water is 100-200000mg/L, is preferably 300-150000mg/L.
The present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention, can carry out multiple simple variant to technical scheme of the present invention, and these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out arbitrary combination between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
To be further described in detail embodiments of the invention below.
In following embodiment, the measuring method of the COD of waste water is dichromate titration (GB11914-89), and the measuring method of BOD is dilution inoculation method (GB/T 7488-1987).The measuring method of useless electrical conductivity of water adopts glass electrode method (GB/T 18570.9-2005), and the measuring method of chlorion adopts silver nitrate titration method (GB11896-89).
Embodiment 1
The present embodiment is for illustrating the treatment process of saliferous provided by the invention, chloride ion-containing waste water.
The waste water of the present embodiment processing is adopted waste water for certain oil field three, and described useless electrical conductivity of water is 9000 μ s, and chlorine ion concentration is 2000mg/L.
The pH value of above-mentioned pending waste water is adjusted to 4 with aqueous sulfuric acid (mass percent concentration is 98%), (anode is SnO to be placed in electrochemical reactor
2/ Ti, negative electrode is stainless steel; Strength of current is 200A/m
2); and add metal ion catalyst iron protochloride (in described ferrous ion and waste water, the mol ratio of chlorion is 0.05: 1) and catalyst protective agent ethylenediamine tetraacetic acid (EDTA) and citric acid (mass ratio is 2: 1) (mass ratio of catalyzer and catalyst protective agent is 1: 0.5) in described waste water; and mix, the residence time in described electrochemical reactor is 40 minutes.
The above-mentioned pH value through electrochemical catalytic oxidation waste water after treatment is adjusted to 6.5 with aqueous sodium hydroxide solution (mass percent concentration is 30%), and is placed in flocculation basin and carries out gravity settling, to carry out solid-liquid separation, the residence time is 20 minutes.Waste water quality index before and after processing is as shown in table 1.
Comparative example 1
This comparative example is for illustrating the reference method of wastewater treatment.
Process waste water according to the method for embodiment 1, different, in waste water, do not add catalyst protective agent, and the add-on of catalyzer iron protochloride changes (in described ferrous ion and waste water, the mol ratio of chlorion is 0.1: 1).Waste water quality index before and after processing is as shown in table 1.
Table 1
| Waste water quality index | COD(mg/L) | B/C |
| Before processing | 600 | 0.01 |
| Comparative example 1 | 100 | 0.23 |
| Embodiment 1 | 90 | 0.38 |
From the results shown in Table 1, adopt the clearance of the COD of method of the present invention waste water after treatment to reach 85%, and the COD clearance of comparative example 1 is only 83%; Adopt the B/C ratio of method of the present invention waste water after treatment to reach 0.38, and comparative example 1 is only 0.23, and the amount of the catalyzer that adds of method of the present invention still less.
Embodiment 2
The present embodiment is for illustrating the treatment process of saliferous provided by the invention, chloride ion-containing waste water.
The waste water of the present embodiment processing is the electric desalting waste water of certain refinery, and described useless electrical conductivity of water is 8000 μ s, and chlorine ion concentration is 1800mg/L.
The pH value of above-mentioned pending waste water is adjusted to 5 with aqueous hydrochloric acid (mass percent concentration is 30%), (anode is PbO to be placed in electrochemical reactor
2/ Ti, negative electrode is stainless steel; Strength of current is 150A/m
2); and add catalyzer iron protochloride (in described ferrous ion and waste water, the mol ratio of chlorion is 0.01: 1) and catalyst protective agent ethylenediamine tetraacetic acid (EDTA) and oxalic acid (mass ratio is 3: 1) (mass ratio of catalyzer and catalyst protective agent is 1: 0.08) in described waste water; and mix, the residence time in described electrochemical reactor is 60 minutes.
The above-mentioned pH value through electrochemical catalytic oxidation waste water after treatment is adjusted to 7 with aqueous sodium carbonate (mass percent concentration is 35%), and is placed in flocculation basin and carries out gravity settling, to carry out solid-liquid separation, the residence time is 20 minutes.Waste water quality index before and after processing is as shown in table 2.
Comparative example 2
This comparative example is for illustrating the reference method of wastewater treatment.
Process waste water according to the method for embodiment 2, different, in waste water, do not add catalyst protective agent, and the add-on of catalyzer iron protochloride changes (in described ferrous ion and waste water, the mol ratio of chlorion is 0.08: 1).Waste water quality index before and after processing is as shown in table 2.
Table 2
| Waste water quality index | COD(mg/L) | B/C |
| Before processing | 730 | 0.05 |
| Comparative example 2 | 175 | 0.22 |
| Embodiment 2 | 124 | 0.37 |
From the results shown in Table 2, adopt the clearance of the COD of method of the present invention waste water after treatment to reach 83%, and the COD clearance of comparative example 1 is only 76%; The B/C ratio of method of the present invention waste water after treatment reaches 0.37, and comparative example 1 is only 0.22, and the amount of the catalyzer that adds of method of the present invention still less.
Embodiment 3
Embodiment is for illustrating the treatment process of waste water provided by the invention.
Process waste water according to the method for embodiment 1; different is; metal ion catalyst used is ferrous sulfate; in metal ion and waste water, the mol ratio of chlorion is 0.1: 1; catalyst protective agent is oxalic acid and citric acid (mass ratio is 1: 2); the mass ratio of catalyzer and catalyst protective agent is 1: 2, and strength of current is 300A/m
2, the residence time is 30 minutes; The COD value of processed waste water is 48mg/L, and the clearance of COD reaches 92%, and the B/C ratio of waste water after treatment reaches 0.36.
Embodiment 4
Embodiment is for illustrating the treatment process of waste water provided by the invention.
Process waste water according to the method for embodiment 2; different is; catalyzer used is Iron nitrate; in metal ion and waste water, the mol ratio of chlorion is 1: 1; catalyst protective agent is ethylenediamine tetraacetic acid (EDTA) and oxalic acid (mass ratio is 1: 1); the mass ratio of catalyzer and catalyst protective agent is 1: 0.8, and strength of current is 500A/m
2, the residence time is 70 minutes; The COD value of processed waste water is 37mg/L, and the clearance of COD reaches 95%, and the B/C ratio of waste water after treatment reaches 0.36.
Embodiment 5
Embodiment is for illustrating the treatment process of waste water provided by the invention.
Process waste water according to the method for embodiment 1, different, described catalyst protective agent is ethylenediamine tetraacetic acid (EDTA) (mass ratio of catalyzer and catalyst protective agent is 1: 0.5); The COD value of processed waste water is 95mg/L, and the B/C ratio of waste water after treatment reaches 0.31.
Embodiment 6
Embodiment is for illustrating the treatment process of waste water provided by the invention.
Process waste water according to the method for embodiment 1; different is; in described waste water, add metal ion catalyst iron protochloride (in described ferrous ion and waste water, the mol ratio of chlorion is 0.005: 1) and catalyst protective agent ethylenediamine tetraacetic acid (EDTA) and nitrilotriacetic acid(NTA) (mass ratio is 2: 1) (mass ratio of catalyzer and catalyst protective agent is 1: 0.03); the residence time in described electrochemical reactor is 95 minutes; the COD value of processed waste water is 96mg/L; the clearance of COD reaches 84%, and the B/C ratio of waste water after treatment reaches 0.36.
Embodiment 7
Embodiment is for illustrating the treatment process of waste water provided by the invention.
Process waste water according to the method for embodiment 1, different, described metal ion catalyst is zinc sulfate.The residence time in described electrochemical reactor is 95 minutes, and the COD value of processed waste water is 96mg/L, and the clearance of COD reaches 84%, and the B/C ratio of waste water after treatment reaches 0.33.
BOD/COD accounts for whole organic shares than biodegradable organism in value representation waste water, and the biodegradable degree of this waste water.Can find out from the result of embodiment 1 to embodiment 7, adopt method of the present invention can significantly improve the value of the B/C of processed waste water, thereby can illustrate, adopt the biodegradability of method of the present invention waste water after treatment to be significantly improved.From relatively can finding out of embodiment 1 and embodiment 5, while adopting the preferred catalyst protective agent of the present invention, water treatment effect is better.From relatively can finding out of embodiment 1 and embodiment 7, while adopting the preferred catalyzer of the present invention, water treatment effect is better.
Claims (12)
1. the treatment process of the waste water of a saliferous, chloride ion-containing, it is characterized in that, the method comprises carries out described waste water, catalyzer and catalyst protective agent combination treatment under electrochemical catalytic oxidation condition, the B/C > 0.3 that makes waste water after treatment, then carries out solid-liquid separation by waste water after treatment; Described catalyzer is metal ion catalyst; Described catalyst protective agent can improve the utilization ratio of catalyzer, and described catalyst protective agent is selected from any two kinds in ethylenediamine tetraacetic acid (EDTA), nitrilotriacetic acid(NTA), oxalic acid and citric acid, and the mass ratio of any two kinds is 0.1-10:1.
2. method according to claim 1; wherein; the method of described combination treatment comprises described waste water, catalyzer and catalyst protective agent is placed in to the electrochemical reactor with anode and negative electrode; connect the anode of described reactor and the power supply of negative electrode, waste water, catalyzer and catalyst protective agent are carried out under electrochemical catalytic oxidation condition to combination treatment.
3. method according to claim 1 and 2, wherein, described electrochemical catalytic oxidation condition comprises that strength of current is 0.1-1000A/m
2; The time of combination treatment is 10-90 minute.
4. method according to claim 3, wherein, described strength of current is 1-500A/m
2; The time of described combination treatment is 30-60 minute.
5. method according to claim 2, wherein, described anode is selected from SnO
2/ Ti, PbO
2one in/Ti, Pt, graphite, active carbon fibre peacekeeping stainless steel; Described negative electrode is stainless steel electrode.
6. method according to claim 1 and 2, wherein, the pH value of described waste water is 1-7.
7. method according to claim 1, wherein, the mol ratio of the chlorion in metal ion and waste water in described metal ion catalyst is 0.001-10:1.
8. method according to claim 7, wherein, in the metal ion in described metal ion catalyst and waste water, the mol ratio of chlorion is 0.005-5:1.
9. method according to claim 1, wherein, the mass ratio of described metal ion catalyst and described catalyst protective agent is 1:0.03-10.
10. method according to claim 9, wherein, the mass ratio of described metal ion catalyst and described catalyst protective agent is 1:0.05-2.
11. methods according to claim 1, wherein, the metal in described metal ion catalyst is selected from one or more in Fe, Mn, Ni, Co, Cd, Cu, Ag, Cr and Zn.
12. methods according to claim 1 and 2, wherein, described useless electrical conductivity of water is 500-200000 μ s, the chlorine ion concentration in described waste water is 300-200000mg/L.
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| US9340436B2 (en) * | 2013-04-16 | 2016-05-17 | Palo Alto Research Center Incorporated | Sea water desalination system |
| CN105016431A (en) * | 2015-07-23 | 2015-11-04 | 王麒钧 | Method and apparatus for removal and recovering of heavy metal ions from wastewater |
| CN108726740A (en) * | 2018-06-11 | 2018-11-02 | 山东龙安泰环保科技有限公司 | A kind of high sodium chloride waste water Zero discharge treatment method |
| CN116462303B (en) * | 2023-04-28 | 2024-08-16 | 湖南中天元环境工程有限公司 | Catalytic wet oxidation compound homogeneous catalyst and preparation method and application thereof |
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| CN101092573A (en) * | 2006-06-22 | 2007-12-26 | 中国石油化工股份有限公司 | A hydrogenation method for producing diesel oil in low sulphur |
| CN101723486A (en) * | 2008-10-23 | 2010-06-09 | 中国石油化工股份有限公司 | Method for treating salt-and-chlorine-contained wastewater |
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| EP1170259A1 (en) * | 2000-07-05 | 2002-01-09 | Sony International (Europe) GmbH | Electrochemical apparatus and process for purification of fluids |
| CN100553768C (en) * | 2006-05-12 | 2009-10-28 | 中国科学院大连化学物理研究所 | A kind of loaded and non-supported catalyst and preparation method |
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| CN101092573A (en) * | 2006-06-22 | 2007-12-26 | 中国石油化工股份有限公司 | A hydrogenation method for producing diesel oil in low sulphur |
| CN101723486A (en) * | 2008-10-23 | 2010-06-09 | 中国石油化工股份有限公司 | Method for treating salt-and-chlorine-contained wastewater |
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