CN105036424B - A kind of waste water desalination purification method of recycling and its application - Google Patents
A kind of waste water desalination purification method of recycling and its application Download PDFInfo
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Abstract
The invention discloses a kind of waste water desalination purification method of recycling and its application, wherein purification method comprises the following steps：(1) salt-containing organic wastewater is handled using Bipolar Membrane, obtains the aqueous solution containing organic matter, and acid solution and alkaline solution；(2) in pH=2~12, pressure is 2~8MPa, under conditions of temperature is 180~300 DEG C, to carrying out wet oxidation containing organic solution, obtains treatment fluid；(3) treatment fluid is carried out post-processing to obtain water outlet.Before processing is carried out using Bipolar Membrane to salt-containing organic wastewater to filter in advance.The method provided by the invention for handling salt-containing organic wastewater using Bipolar Membrane and wet oxidation, can significantly reduce the COD value of waste water, while the material in waste water is effectively recycled.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of waste water desalination purification method of recycling and its should
With.
Background technology
In chemical process, many salt-containing organic wastewaters are inevitably produced, such as H acid waste water, T acid waste water, J acid
Waste water, DSD acid waste water etc., in order to meet the needs of environmental protection, it is necessary to handle these waste water, to reach discharge mark
It is accurate.
Such as：Main organic pollution in H acid waste water is naphthalene and naphthalene derivative, and host inorganic thing is sodium sulphate and ammonium
Salt, and compared to the waste water of other organic matters of system containing naphthalene, there is its particularity：
(1) pollutant component is complicated, and concentration is high, the H- acid mother liquors discharged in process of production, derives containing a large amount of naphthalene systems
Thing, COD are up to tens of thousands of mg/L, complicated component；
(2) acid strong, pH is about between 1~2；
(3) colourity is deep, and about 1 × 105Left and right, typically in pale brown to dark brown；
(4) toxicity is big, and H acid belongs to condensed-nuclei aromatics, has strong bio-toxicity, if waste water directly discharges without processing,
Environment will be seriously polluted, also there is very big harm to human body；
(5) not easily biological-degradable, because the conjugatedπbond for the delocalization that naphthalene nucleus is made up of 10 carbon atoms, structure are quite steady
It is fixed, it is difficult to degrade.
T acid producing waste waters belong to difficult waste water from dyestuff, waste water COD respectively in 70000mg/L or so, colourity is deep, into
Divide complexity, toxicity is big, salt content is high, acid strong, it is impossible to directly carry out biochemical treatment.
The mode of existing processing industrial wastewater is varied, is reduced by various physical chemistry and biological means in waste water
Pollutant load, for example, existing H acid isolation waste water processing method be：First, H acid isolation waste water is extracted；So
Afterwards, carry out concentrating salt steaming, obtained sodium sulphate does fixed-end forces or reuse.Due to the excess production capacity of sodium sulphate, and concentrate salt
The sodium sulfate salt inferior quality that the cost of steaming is high, obtains, application are narrow.
The content of the invention
The invention provides a kind of waste water desalination purification method of recycling, the COD value of waste water can be significantly reduced, simultaneously
Material in waste water is effectively recycled.
A kind of waste water desalination purification method of recycling, comprises the following steps：
(1) salt-containing organic wastewater is handled using Bipolar Membrane, obtains the aqueous solution containing organic matter, and acid solution
And alkaline solution；
(2) in pH=2~12, pressure is 2~8MPa, under conditions of temperature is 180~300 DEG C, to containing organic solution
Wet oxidation is carried out, obtains treatment fluid；
(3) treatment fluid is carried out post-processing to obtain water outlet.
A small amount of acid or alkali can be included in salt-containing organic wastewater of the present invention, method provided by the invention is applied to equal
Organic brine waste of phase, it is particularly suitable for the processing for producing waste water of naphthalene sulfonic acids class, heterocyclic (such as indoles) product, example
Such as：Caused waste water in H acid, the production process such as T acid, tobias acid, J acid, Sulpho Tobias Acid, K acid, γ acid, it is useless for H acid isolations
During water, COD clearance is up to more than 95%.
Method provided by the invention can use industrial continuous production, i.e. salt-containing organic wastewater is successively gone through successively
The processing procedure of step (1)~step (3), obtains standard compliant processing water.
Bipolar Membrane issues unboiled water dissociation in electric field action, produces H+And OH-Ion, and bipolar membrane electrodialysis technology is by this
Kind specific function is combined in common electrodialysis, so as to realize production/regeneration of instant acid/base, or acidifying and/or alkali
Change.If bipolar membrane electrodialysis technology is applied in salt-containing organic wastewater, it can not only make waste water desalination, and the bronsted lowry acids and bases bronsted lowry generated
It can be back in production or waste water subsequent treatment.
Method provided by the invention, first industrial wastewater (i.e. the organic wastewater of saliferous) is reclaimed to obtain by Bipolar membrane water splitting
Organic matter degradation is small molecule, after then passing through through wet oxidation by acid solution and alkaline solution, the organic liquid waste after processing
Processing, obtains clean pure water, completes the processing of waste water.
Wet oxidation is the efficient oxidation technology under a kind of HTHP, has a wide range of application and treatment effeciency is high, will can be given up
Larger molecular organicses in water, which decompose, is oxidized to the further removal such as small molecule organic carboxyl acid, alcohols, amine, or carbon dioxide,
Sulfur dioxide, ammonia, nitrogen etc. are excluded or absorbed.But the inorganic salts (such as nitrate, sulfate, halide salt etc.) in waste water
Corrosion phenomenon can be produced to wet oxidation reaction kettle, reduce reactor service life, improve operating cost.
Waste water is subjected to desalination by Bipolar Membrane first, corrosion of the salt to wet oxidation reaction kettle is not only reduced, drops
Low cost, it can also prepare using the clean bronsted lowry acids and bases bronsted lowry more extensive, value is bigger.
The present invention have studied the composition and characteristic of salt-containing organic wastewater, the pros and cons of existing processing method be analyzed, using double
The combination of pole EDBM technology and Wet Oxidation Process and other treatment technologies, has not only reclaimed salt, additionally it is possible to will
COD value in waste water substantially reduces.
Filtered in advance preferably, carrying out before processing to salt-containing organic wastewater using Bipolar Membrane.
Before salt-containing organic wastewater enters bipolar membranous system, first filtered, it is solid to remove suspension and iron, calcium, magnesium etc.
Body material.
Preferably, the treatment conditions of Bipolar Membrane are in step (1)：The voltage of single film<2.5V, current density 100
~600A/m2, temperature is 1~40 DEG C.
Film in bipolar membrane electrodialysis system mainly has cavity block, anode membrane, Bipolar Membrane.Salt in salt-containing organic wastewater and acid or
Alkali directional migration in the presence of electric field, when running into zwitterion film in transition process, selectivity occurs and passes through.Run into anode membrane
When, cation is by the way that anion is trapped；When running into cavity block similarly；When running into Bipolar Membrane, the band opposite sex discharged with film table is electric
Ion (the H of lotus+Or OH-) combine, generation acid or alkali.Under electric field action, the ion in waste water all migrates out from waste water, with H+Or OH-With reference to generation soda acid, the salt in waste water is fully recycled, salt content is relatively low in the waste water after processing, to wet type oxygen
The corrosion for changing reactor is small.
The purpose of wet oxidation reduces COD value, due to wet oxidation in being small molecule by the organic matter degradation in solution
Condition it is more harsh, use, equipment caused damage for a long time inevitably, it is excellent in order to take into account the effect of wet oxidation
Selection of land, the time of wet oxidation is 2~6h in step (2).
Further preferably, the pH of wet oxidation is 4~10, and pressure be 5~8MPa, and temperature is 200~280 DEG C, during reaction
Between be 2~4h.Further preferably, the pH of wet oxidation is 6~10, and pressure is 5~7MPa, and temperature is 200~250 DEG C, the reaction time
For 2~4h.
COD value significantly reduces after wet oxidation, urges obtaining treatment fluid and is post-processed, the post processing for flocculation and/or
Decolourize.If post processing selection is decolourized, it is preferable that the decolorising agent is one kind in activated carbon, diatomite, aluminum oxide, molecular sieve
It is or several..
Preferably, the waste water before wet oxidation is pre-processed.Pretreatment uses light electrolysis and/or diazonium.Micro- electricity
Nitrose material can be reduced into amine by solution, and nitrite can generate diazonium product with amine reaction, and amine and diazonium product are more
Easy wet oxidation, the small molecule for aoxidizing generation are ammonia, ammonium salt or nitrogen, safer, easy removal.
Preferably, being flocculated after light electrolysis, or flocculated after wet oxidation.
Preferably, pretreatment is carried out in bipolar membrane electrodialysis before processing, or after bipolar membrane electrodialysis processing.It is micro-
Electrolysis pretreatment is when bipolar membrane electrodialysis before processing is carried out, it is necessary to after Bipolar Membrane after flocculation filtration iron removaling.
Processing after wet oxidation is post processing, and the post processing is flocculation and/or decolourizes.
Decolourized according to adsorbent, the addition of adsorbent is the 0.05~0.5% for the treatment of fluid quality.Add adsorbent it
Before, pH value is adjusted to 6~8.
According to processing method of the present invention, the production technology of H acid and other products can be improved, below with H
Illustrate exemplified by acid
H acid production processes after improvement are：Refined naphthalene is sulfonated successively, nitrifies, neutralizes, reducing, the sour isolations of T, alkali fusion, H acid
H acid is prepared in isolation, waste water filtered and bipolar film process successively caused by H acid isolations, obtains sulfuric acid and sodium hydroxide, is somebody's turn to do
Sulfuric acid and sodium hydroxide are back in industrial production.For example, sulfuric acid reuse to H acid is isolated into workshop section, sodium hydroxide reuse to alkali
Molten workshop section and/or nitrification workshop section.
After bipolar film process, acid solution and alkaline solution are obtained, for H acid isolation waste water, obtains sulphur
Acid and sodium hydrate aqueous solution.Sulfuric acid solution can be used to prepare bottom water, and (the bottom water used during H acid isolations is that mass fraction is 15-
20% dilute sulfuric acid).Sodium hydroxide solution (nitrified after can be used for the denitrification process of nitrification workshop section, or concentration for alkali fusion
Caused nitrosylsulfuric acid produces a large amount of nitrogen oxides tail gas after adding water in journey, absorbs the tail gas using the aqueous slkali being recovered to,
The nitrite solution of generation can be used for diazo reaction).
The isolation workshop section of H acid production processes of the prior art can produce substantial amounts of waste water, containing a large amount of in these waste water
Sodium sulphate, waste water are handled using Bipolar Membrane after filtering, can obtain sulfuric acid (i.e. acid solution) and sodium hydroxide solution
(i.e. alkaline solution), sodium hydroxide solution are used for alkali fusion after can be used for the denitrification process of nitrification workshop section, or concentration.Sulfuric acid solution
It can be used to prepare bottom water.
Waste water filtered and bipolar film process successively caused by T acid isolations, obtains sulfuric acid and ammoniacal liquor, sulfuric acid and ammoniacal liquor reuse
In industrial production.When sulfuric acid and ammoniacal liquor are carrying out reuse, it can be further processed according to specific needs, with up to
To the requirement of recycling.Such as sulfuric acid and ammoniacal liquor are concentrated, reuse can be distinguished to H acid isolation workshop section and neutralize workshop section.
The present invention compared with prior art, has the advantages that：
(1) processing method provided by the invention can significantly reduce the COD value in waste water, COD clearance 96% with
On；
(2) processing method provided by the invention uses bipolar film process, obtained bronsted lowry acids and bases bronsted lowry reuse to industry life to waste water
In the corresponding workshop section of production, the utilization rate of raw material is improved.
(3) processing method provided by the invention is suitable to continuous production, is easy to industrially popularization and application.
Embodiment
Embodiment 1
H acid waste water, in black, COD=26030mg/L, pH=2.
(1) H acid waste water is filtered, to remove the material such as suspension and iron, calcium, magnesium；
(2) bipolar film process：Using bipolar film process filtrate, alkaline solution and mass fraction are obtained as 10% sulfuric acid,
The mass fraction of sodium hydroxide is 4% in alkaline solution, and the mass fraction of ammonia is 4%.The condition of Bipolar Membrane is：Individual membrane voltage
For 2.0V, current density 600A/m2, temperature is 30 DEG C, processing time 120min.
(3) wet oxidation：The pH of the solution containing organic matter obtained after bipolar film process is adjusted to 7, then squeezed into wet
In formula stills for air blowing, 250 DEG C, pressure 6MPa are warming up to, is cooled after being passed through air oxidation 2h.
Measure out kettle waste water and show orange-yellow, pH=4.5, COD=2083mg/L, NH3- N=164.2mg/L.
(4) adsorb：The kettle waste water that goes out of step (3) is adjusted to neutral pH=7, adds mass fraction as 0.1% (with regulation
On the basis of the quality of waste water after pH) activated carbon stirring and adsorbing 0.5h after filter, obtained filtrate is in slightly yellow, then adds quality
Fraction be 0.1% activated carbon (on the basis of the quality of the waste water after adjusting pH) stirring and adsorbing 0.5h after be filtrated to get almost without
The transparent filtrate of color, COD=150mg/L, salt content 4%.
Embodiment 2
H acid waste water, in black, COD=26030mg/L, pH=2.
(1) H acid waste water is filtered, to remove the material such as suspension and iron, calcium, magnesium；
(2) bipolar film process：Using bipolar film process filtrate, alkaline solution and mass fraction are obtained as 9% sulfuric acid, alkali
Property solution in the mass fraction of sodium hydroxide be 3.9%, the mass fraction of ammonia is 3.5%.The condition of Bipolar Membrane is single film electricity
Press as 1.5V, current density 400A/m2, temperature is 30 DEG C, processing time 100min.
(3) wet oxidation：The pH of the solution containing organic matter obtained after bipolar film process is adjusted to 8, then squeezed into wet
In formula stills for air blowing, 250 DEG C, pressure 6MPa are warming up to, is cooled after being passed through air oxidation 1.5h.
Measure out kettle waste water and show orange-yellow, pH=4.5, COD=2483mg/L, NH3- N=165.0mg/L.
(4) adsorb：Step (3) go out in kettle waste water add mass fraction be 0.2% activated carbon (to go out kettle waste water
On the basis of quality) stirring and adsorbing 30min, filter and obtain yellowish treatment fluid, its COD=1545mg/L.
Embodiment 3
H acid waste water, in black, COD=130000mg/L, pH=1.
(1) H acid waste water is filtered, to remove the material such as suspension and iron, calcium, magnesium；
(2) bipolar film process：Using bipolar film process filtrate, alkaline solution and mass fraction are obtained as 11% sulfuric acid,
The mass fraction of sodium hydroxide is 4.5% in alkaline solution, and the mass fraction of ammonia is 4.5%.The condition of Bipolar Membrane is single film
Voltage is 1.5V, current density 600A/m2, temperature is 30 DEG C, processing time 120min.
(3) wet oxidation：The pH of the solution containing organic matter obtained after bipolar film process is adjusted 7, then adds high pressure
In kettle, 30atm air is passed through, is cooled after being reacted one hour at 250 DEG C；
Pressure release after cooling, the air for being further continued for being passed through 30atm continue to cool after reacting one hour at 250 DEG C；
After cooling pressure release, then 30atm air is passed through, is reacted 1.5 hours at 250 DEG C.Water outlet yellow, COD=
6500mg/L, COD clearance 95%.
(4) decolourize：The activated carbon that addition mass fraction is 0.3% into the water outlet of step (3) is (with the water outlet of step (3)
On the basis of quality) filter after stirring and adsorbing 30min, then filtered after adding the charcoal absorption that mass fraction is 0.1%, filtrate is shallow
Yellow, survey COD=6545mg/L.
Comparative example 1
It is that step (4) uses ClO with the difference of embodiment 32Decolourize, concrete operations are as follows：
0.2% ClO is added in water outlet to step (3)2(ClO2Dosage on the basis of the quality of waste water), under normal temperature
30min is reacted, after adding activated carbon (on the basis of effluent characteristics of step (3)) the absorption 30min that mass fraction is 0.1%
Filter, color is crocus, and decolorizing effect is undesirable.
Comparative example 2
It is that step (4) is decolourized using Fe/C with the difference of embodiment 3, concrete operations are as follows：
The water outlet pH=4 of pacing rapid (3), adds that mass fraction is 0.2% activated carbon and mass fraction is 2% iron powder (with step
Suddenly on the basis of the effluent characteristics of (3)) filter after reaction 4h, then pH=8 is adjusted to, is filtered after the 30min that flocculates, filtrate is crocus,
Decolorizing effect is undesirable.
Embodiment 4
(1) refined naphthalene is sulfonated successively, nitrifies, neutralize, reducing, the sour isolations of T, alkali fusion, H acid isolate and H acid is prepared.
(2) H acid isolation waste water is filtered, to remove the material such as suspension and iron, calcium, magnesium；
(3) bipolar film process：Using the filtrate of Bipolar Membrane processing step (2), obtain alkaline solution and mass fraction is
9.8% sulfuric acid, the mass fraction of sodium hydroxide is 3.7% in alkaline solution, and the mass fraction of ammonia is 3.7%.Bipolar Membrane
Condition is that individual membrane voltage is 1.5V, current density 450A/m2, temperature is 30 DEG C, processing time 120min.
By sulfuric acid reuse obtained by the step to H acid isolations workshop section, gained alkaline solution is rotated, obtains sodium hydroxide
Reuse is to alkaline melt workshop section.
(4) wet oxidation：The pH of the solution containing organic matter obtained after step (3) bipolar film process is adjusted to 7, then
Squeeze into wet oxidation kettle, be warming up to 250 DEG C, pressure 6MPa, cool after being passed through air oxidation 1.5h.
Measure out kettle waste water and show orange-yellow, pH=4.5, COD=2107mg/L.
(5) adsorb：Step (4) go out in kettle waste water add mass fraction be 0.3% activated carbon (to go out kettle waste water
On the basis of quality) absorption 30min, filter and obtain flaxen treatment fluid, then adjust pH to 6.0, color is changed into yellow, then adds
The activated carbon (on the basis of going out the quality of kettle waste water) that mass fraction is 0.2% adsorbs 30min, and suction filtration obtains yellowish processing
Liquid, its COD=1487mg/L.
(6) T acid isolation waste water is filtered, to remove the material such as suspension and iron, calcium, magnesium；
(7) bipolar film process：Using the filtrate of Bipolar Membrane processing step (6), obtain alkaline solution and mass fraction is
9.8% sulfuric acid, by the sulfuric acid reuse to T acid isolations workshop section.The condition of Bipolar Membrane is that individual membrane voltage is 1.5V, current density
For 450A/m2, temperature is 30 DEG C, processing time 120min.
(8) wet oxidation：The pH of the solution containing organic matter obtained after step (7) bipolar film process is adjusted to 8, added
Mass fraction is 0.5% CuSO4·5H2O is as catalyst (on the basis of T acid isolation wastewater qualities), in 260 DEG C of temperature, pressure
3h is reacted under the conditions of power 7MPa, reaction filters after terminating and obtains the filtrate (i.e. filtrate I) of chartreuse, its pH=2.1 or so,
COD clearances are 85%.
(9) FeSO that mass fraction is 0.5% is added into filtrate I4·7H2O (on the basis of T acid isolation wastewater qualities),
Treat FeSO4·7H2After O is completely dissolved, adds the liquid caustic soda that mass fraction is 5.5% and adjust pH=8.5, flocculate 30min, filters
To the filtrate II of blueness.
(10) Na that mass fraction is 0.6% is added in filtrate II2S·9H2O is (using T acid isolation wastewater qualities as base
It is accurate), react 30min, remove complex copper, suction filtration obtains filtrate III as black (CuS particles are smaller, partly into filtrate).
(11) in filtrate III add the concentrated sulfuric acid readjustment pH=6.0, additions mass fraction for 0.2% activated carbon (with T acid from
On the basis of analysis wastewater quality) absorption 30min, subdiaphanous filtrate is obtained, its COD clearance is 96%.
Claims (5)
1. the waste water desalination purification method of a kind of recycling, it is characterised in that comprise the following steps：
(a) waste water is pre-processed using light electrolysis；
(b) waste water after pretreatment is flocculated；
(1) salt-containing organic wastewater after flocculation is handled using Bipolar Membrane, obtains the aqueous solution containing organic matter, and it is acid
Solution and alkaline solution；Described salt-containing organic wastewater is naphthalene sulfonic acids class, the production waste water of heterocyclic product；
(2) in pH=4~10, pressure is 5~8MPa, under conditions of temperature is 200~280 DEG C, to being carried out containing organic solution
2~4h of wet oxidation, obtains treatment fluid；
(3) treatment fluid is carried out post-processing to obtain water outlet；To be decolourized using adsorbent, the addition of adsorbent is for described post processing
The 0.05~0.5% for the treatment of fluid quality.
2. the waste water desalination purification method of recycling as claimed in claim 1, it is characterised in that have using Bipolar Membrane to saliferous
Machine waste water carries out before processing and filtered in advance.
3. the waste water desalination purification method of recycling as claimed in claim 1, it is characterised in that Bipolar Membrane in step (1)
Treatment conditions are：The voltage of single film<2.5V, current density are 100~600A/m2, temperature is 1~40 DEG C.
4. a kind of production technology of improved H acid, refined naphthalene is sulfonated successively, nitrifies, neutralizes, reducing, the sour isolations of T, alkali fusion, H acid
H acid is prepared in isolation, it is characterised in that waste water is using the money as described in any one of claims 1 to 3 caused by H acid isolations
The waste water desalination purification method in source is handled, and obtains sulfuric acid and sodium hydroxide, the sulfuric acid and sodium hydroxide are back to industry
In production.
5. the production technology of improved H acid as claimed in claim 4, it is characterised in that waste water is using such as caused by T acid isolations
The waste water desalination purification method of recycling described in any one of claims 1 to 3 is handled, and obtains sulfuric acid and ammoniacal liquor, sulfuric acid
It is back to ammoniacal liquor in industrial production.
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| CN105566176B (en) * | 2015-11-26 | 2018-06-22 | 浙江奇彩环境科技股份有限公司 | A kind of production technology of the sour oxysome of improved 6- nitros -1,2,4 |
| CN105236631B (en) * | 2015-11-27 | 2017-09-19 | 福建创源环保有限公司 | A high-salt industrial wastewater treatment method based on multi-electrode and multi-diaphragm electrolyzer |
| CN106587494A (en) * | 2016-12-06 | 2017-04-26 | 浙江力禾集团有限公司 | Method for improving ammonia-nitrogen content of H acid wastewater |
| CN106830492B (en) * | 2017-04-05 | 2021-04-20 | 利民化学有限责任公司 | Treatment method of methoxy acrylic ester pesticide product wastewater |
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| CN102910853A (en) * | 2011-08-03 | 2013-02-06 | 浙江龙盛化工研究有限公司 | Method for producing naphthalene-based superplasticizer by using H acid wastewater recovered solution |
| CN104150722A (en) * | 2014-09-04 | 2014-11-19 | 北京赛科康仑环保科技有限公司 | Treatment process for acrylic fiber waste water |
| CN104261591A (en) * | 2014-10-08 | 2015-01-07 | 上海博丹环境工程技术有限公司 | Method and system for treating high-concentration salt-containing wastewater from prochloraz aminating working section |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102910853A (en) * | 2011-08-03 | 2013-02-06 | 浙江龙盛化工研究有限公司 | Method for producing naphthalene-based superplasticizer by using H acid wastewater recovered solution |
| CN104150722A (en) * | 2014-09-04 | 2014-11-19 | 北京赛科康仑环保科技有限公司 | Treatment process for acrylic fiber waste water |
| CN104261591A (en) * | 2014-10-08 | 2015-01-07 | 上海博丹环境工程技术有限公司 | Method and system for treating high-concentration salt-containing wastewater from prochloraz aminating working section |
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Address after: 312000 Zhejiang province Shaoxing Shunjiang Road No. 683 building 903 room 9 Applicant after: ZHEJIANG QICAI ENVIRONMENT TECHNOLOGY CO., LTD. Address before: Shaoxing City, Zhejiang province 312000 smartfortune Di Dang new building 17 floor room 1709 Applicant before: The extraordinary splendour environmental science and technology company limited in Zhejiang |
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