CN105565566B - A kind of method of Fenton processing 6- nitro -1,2,4- acid oxysome waste water co-production sodium sulphate - Google Patents
A kind of method of Fenton processing 6- nitro -1,2,4- acid oxysome waste water co-production sodium sulphate Download PDFInfo
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Abstract
The invention discloses a kind of methods that Fenton handles 6- nitro-1,2,4-sulfonic acid waste water co-production sodium sulphate, include the following steps：(1) alkali is added to adjust its pH value to 2.0~3.0 into 6- nitro -1,2,4- acid oxysome waste water；(2) under stirring condition, activated carbon, FeSO are added into the waste water for mix up pH value4And H2O2Carry out oxidation reaction；(3) alkali is added to adjust its pH to 9~10 into the waste water after oxidation；(4) Al is added into step (3) processed waste water under stirring2(SO4)3Filtrate is obtained by filtration to the turbid until reaction system pH to 6~7, sufficient standing settle to obtain turbid in solution；(5) if the filtrate that step (4) obtains reaches processing requirement, be concentrated by evaporation, dry after obtain technical grade sulfuric acid sodium；If the filtrate that step (4) obtains is not up to processing requirement, repeatedly step (2)~(4), until reaching processing requirement.The processing method is simple for process, free from environmental pollution, can be reached resource with co-producing sodium sulfate and maximally utilized simultaneously in processing.
Description
Technical field
The invention belongs to the Industrial Wastewater Treatment of environmental protection and reuse technology fields, and in particular to 6- nitros -1,2,4-
The waste water integrated treatment generated in sour oxysome production process, while co-producing sodium sulfate, belong to clean manufacturing scope.
Background technology
6- nitro-1,2,4-sulfonic acids, No. CAS is 5366-84-7, and shown in structure such as formula (I), Chinese nickname is 6- nitre
Base -1-diazo-2-naphthol-4-sulfonic acid is a kind of important dyestuff intermediate, mainly for the manufacture of acid dyes and metal complex
Dyestuff.
The production method of 6- nitro-1,2,4-sulfonic acids by nitrosation, sulfonation, is gone back using ethyl naphthol as primary raw material
The processes such as former indexing, diazotising, acid out, nitrification are prepared.Mainly there are three sources for waste water in production process：(1) it restores
Indexing；(2) acid out；(3) it nitrifies, wherein nitration waste water can the reuse in sulfonation and acid out.What reduction indexing and acid out generated
Waste water main component is naphthalene derivative, and composition is complicated, contains gas chromatography, and acidity is 5~8%, and salinity is 8~15, color
Degree is 15000~35000 times, and COD is 10000~20000mg/L, belongs to high concentration, highly acidity, high salinity, dark shade, difficult drop
The organic wastewater of solution.
There are mainly two types of the methods for handling such waste water at present：(1) complexing abstraction, complexometric extraction processing have efficient
Property, highly selective but accumulative with the impurity in stripping process due to extracting, extraction efficiency reduces after multiple circular treatment, simultaneously
Strip liquor is difficult.(2) traditional Fenton facture, traditional Fenton oxidation technology are mainly excessive by being neutralized with lime
Acid generates the precipitations such as calcium sulfate, and Adsorption organic matter, although percent of decolourization > 90% can be realized, organic matter removal rate is relatively low
(COD removal rates about 60%-70%), and H2O2Utilization rate is relatively low to cause processing cost high, finally goes out because oxidation is not thorough
Water is difficult to make discharged wastewater met the national standard to brown in brown color, it more difficult to reach reuse requirement, and generate a large amount of solid waste, carry
High enterprise's production cost, impacts environment.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of Fentons to handle 6- nitro-1,2,4-sulfonic acid co-productions
The method of sodium sulphate, this method is simple for process, free from environmental pollution, can reach resource maximum with co-producing sodium sulfate simultaneously in processing
Change and utilizes.
A kind of method of Fenton processing 6- nitro-1,2,4-sulfonic acid waste water co-production sodium sulphate, includes the following steps：
(1) alkali is added to adjust its pH value to 2.0~3.0 into 6- nitro -1,2,4- acid oxysome waste water；
(2) activated carbon, FeSO is added under stirring into the waste water for mix up pH value4And H2O2Carry out oxidation reaction；
(3) alkali is added to adjust its pH to 9~10 into the waste water after oxidation；
(4) Al is added into step (3) processed waste water under stirring2(SO4)3Solution, until reaction system pH to 6~
7, sufficient standing settles to obtain turbid, and filtrate is obtained by filtration to the turbid；
(5) if the filtrate that step (4) obtains reaches processing requirement, be concentrated by evaporation, dry after obtain technical grade sulfuric acid sodium；
If the filtrate that step (4) obtains is not up to processing requirement, repeatedly step (2)~(4), until reaching processing requirement.
Preferably, the 6- nitro-1,2,4-sulfonic acid waste water is 6- nitro-1,2,4-sulfonic acid production processes
In, restore the one or two kinds of composite wastes generated in indexing or acid out step.6- nitro -1,2,4- acid oxysomes the production
It refers to using ethyl naphthol as primary raw material, by the production work of nitrosation, sulfonation, reduction indexing, diazotising, acid out, nitrification etc.
Skill.
Preferably, in step (1) and (3), alkali used is solid sodium carbonate or 25~35% sodium hydrate aqueous solutions
One or both of.
Preferably, in step (2), the FeSO that is added4For solid, FeSO4Dosage is that 1~10mmol/L (is referred to
1~10mmol FeSO are added per 1L waste water4)；
The H being added2O2Mass percent concentration is 25~35%, H2O2Dosage is 5~20ml/L.
Preferably, in step (2), activated carbon dosage is 0.5~2g/L, in FeSO4And H2O2It is added before.Wherein,
Activated carbon, which is first added, can make activated carbon fully adsorb organic matter, and row promotes H at carbonium ion center2O2Decompose the hydroxyl generated
The rate and efficiency of free radical cracking organic matter improve H2O2Utilization rate.
Preferably, in step (2), reaction temperature is 25~50 DEG C, and the reaction time is 1~2h, and reactive mode is to stand.
Preferably, in step (4), the Al that is added2(SO4)3Mass percent concentration is 10~30%.
In the present invention, if filtrate does not reach requirement, pH value is adjusted to 2.0~3.0, step (2)~(4) is repeated, adjusts
PH value can use sulfuric acid, can also directly use waste water, and for most of waste water, the number for repeating step (2)~(4) is 2~4
It is secondary.
Preferably, working as liquor C OD≤200mg/L, when coloration≤16 times, reach processing requirement, at this point, obtained sulfuric acid
Sodium purity is high, and waste water is environmentally safe.
Compared with existing Fenton handles the method for organic wastewater, beneficial effects of the present invention are as follows：
(1) the method will restore one or both of indexing or acid out process during 6- nitro -1,2,4- acid oxysome
Composite waste is uniformly processed, and improves waste water treatment efficiency and utilization rate of equipment and installations.
(2) one or two kinds of adjusting waste water in solid sodium carbonate or 25~35% sodium hydrate aqueous solutions are used, lime is not had to
It neutralizes, can not only reduce the generation of solid waste, but also the salinity in waste water can be made single, convenient for recycling.
(3) in FeSO4、H2O2Activated carbon is added before, activated carbon adsorption organic matter, row is convenient for promote at chain carrier
Into H2O2The rate and efficiency of the hydroxyl radical free radical degradation of organic substances generated are decomposed, H is improved2O2Utilization rate.
(4) activated carbon can adsorb the organic matter that water is dissolved in waste water, through settling, filtering, be gone together with organic matter mud
It removes, improves waste water treatment efficiency.And activated carbon can be used as filter aid, improve filtering rate.
(5) with 10~30% Al2(SO4)3, wastewater pH can be not only adjusted back, but also by being generated after adjusting pH to 6~7 again
Flocculant can further remove the organic matter in waste water by sedimentation.
(6) by continuous oxidation, sedimentation, filter process 2~4 times, the color of 6- nitro-1,2,4-sulfonic acid waste water can be realized
Degree, COD efficiently removes that (chroma removal rate reaches 99.9%, COD removal rates more than 98%), and stable effluent quality can pass through
It is concentrated by evaporation, obtains technical grade sulfuric acid sodium after drying.
(7) this method is without being equipped with particular device, it is only necessary to it is relatively simple simple operations, the process flow such as to stir, settle, filter
Single, processing cost is relatively low.
Specific implementation mode
Embodiment 1
The indexable waste water of the 6- nitro-1,2,4-sulfonic acids of 200ml reduction is placed in beaker, with sodium carbonate tune pH to 2.5,
0.3g activated carbons, the FeSO of 1mmol are added at 35 DEG C4, the H that 3ml mass percent concentrations are 28% is then added slowly again2O2, protect
Temperature-resistant, standing reaction 2h is held, is that 25% sodium hydrate aqueous solution adjusts pH to 10 with mass percent, it is slow under stirring to be added
The Al that mass fraction is 10%2(SO4)3Solution adjusts pH to 6.2, stands 0.5h later.Turbid after the standing sedimentation is carried out
Filtering.Repeated oxidation, sedimentation, filter process 3 times, filtrate reach processing requirement, be concentrated by evaporation, it is dry after obtain technical grade sulfuric acid
Sodium, content reach 98% or more.
Embodiment 2
The 6- nitro-1,2,4-sulfonic acid acid out waste water of 200ml is placed in beaker, with sodium carbonate tune pH to 2.0,45 DEG C
Lower addition 0.4g activated carbons, the FeSO of 2mmol4, the H that 4ml mass percent concentrations are 28% is then added slowly again2O2, keep temperature
Constant, standing reaction 1.5h is spent, pH to 9.5 is adjusted with 35% sodium hydrate aqueous solution, mass fraction is added under stirring slowly is
30% Al2(SO4)3Solution adjusts pH to 6.5, stands 1h later.Turbid after the standing sedimentation is filtered.Repeat oxygen
Change, sedimentation, filter process 2 times, filtrate reaches processing requirement, be concentrated by evaporation, it is dry after obtain technical grade sulfuric acid sodium, content reaches
98% or more.
Embodiment 3
6- nitro-1,2,4-sulfonic acids reduction indexing and acid out waste water by each 100ml are placed in beaker, with 30% hydrogen-oxygen
Change sodium tune pH to 2.8,0.1g activated carbons, the FeSO of 0.5mmol is added at 25 DEG C4, it is dense that 2ml mass percents are then added slowly again
The H that degree is 28%2O2, keep temperature-resistant, stand reaction 1.5h, pH to 9.3, stirring are adjusted with 30% sodium hydrate aqueous solution
The lower slow Al that mass fraction is added and is 20%2(SO4)3Solution adjusts pH to 6.5, stands 0.5h later.After the standing sedimentation
Turbid is filtered.Repeated oxidation, sedimentation, filter process 4 times, filtrate reach processing requirement, be concentrated by evaporation, it is dry after obtain work
Industry grade sodium sulphate, content reach 98% or more.
Embodiment 4
6- nitro -1,2,4- acid oxysome the acid outs of the 6- nitro -1,2,4- acid oxysomes reduction indexing of 50ml and 150ml are given up
Water is placed in beaker, and with sodium carbonate tune pH to 2.3,0.3g activated carbons, the FeSO of 1.5mmol are added at 40 DEG C4, then slow again to add
Enter the H that 2ml mass percent concentrations are 28%2O2, keep temperature-resistant, reaction 2h stood, with 25% sodium hydrate aqueous solution tune
PH to 9.8 is saved, the lower slow Al that mass fraction is added and is 30% is stirred2(SO4)3Solution adjusts pH to 6.3, stands 1h later.By institute
Turbid is filtered after stating standing sedimentation.Repeated oxidation, sedimentation, filter process 3 times, filtrate reach processing requirement, be concentrated by evaporation,
Technical grade sulfuric acid sodium is obtained after drying, content reaches 98% or more.
Embodiment 5
6- nitro -1,2,4- acid oxysome the acid outs of the 6- nitro -1,2,4- acid oxysomes reduction indexing of 150ml and 50ml are given up
Water is placed in beaker, and with sodium carbonate tune pH to 2.3,0.2g activated carbons, the FeSO of 2mmol are added at 40 DEG C4, then slow again to be added
The H that 3ml mass percent concentrations are 28%2O2, keep temperature-resistant, stand reaction 1h, adjusted with 35% sodium hydrate aqueous solution
PH to 9.0 stirs the lower slow Al that mass fraction is added and is 20%2(SO4)3Solution adjusts pH to 6.8, stands 1h later.It will be described
Turbid is filtered after standing sedimentation.Repeated oxidation, sedimentation, filter process 3 times, filtrate reach processing requirement, are concentrated by evaporation, are dry
Technical grade sulfuric acid sodium is obtained after dry, content reaches 98% or more.
Comparative example 1
6- nitro-1,2,4-sulfonic acids reduction indexing and acid out waste water by each 100ml are placed in beaker, with 30% hydrogen-oxygen
Change sodium tune pH to 2.8,0.4g activated carbons are added at 25 DEG C, stirring decoloration is filtered, is added in filtrate for 1.5 hours
The FeSO of 0.5mmol4, the H that 2ml mass percent concentrations are 28% is then added slowly again2O2, keep temperature-resistant, stand reaction
1.5h adjusts pH to 9.3 with 30% sodium hydrate aqueous solution, stirs the lower slow Al that mass fraction is added and is 20%2(SO4)3It is molten
Liquid adjusts pH to 6.5, stands 0.5h later.Turbid after the standing sedimentation is filtered.Repeated oxidation, sedimentation, filter process
4 times, filtrate reaches processing requirement, is concentrated by evaporation, obtains technical grade sulfuric acid sodium after drying, testing result is shown in Table 1.
COD, coloration and gained sodium sulphate before and after above example wastewater treatment are surveyed by standard test method
Fixed, testing result is as shown in table 1.
The handling result of table 1 Examples 1 to 5 and comparative example 1
Claims (5)
1. a kind of method of Fenton processing 6- nitro-1,2,4-sulfonic acids production waste water co-production sodium sulphate, which is characterized in that packet
Include following steps：
(1) it is produced in waste water to 6- nitro -1,2,4- acid oxysomes plus alkali adjusts its pH value to 2.0~3.0；
(2) activated carbon and FeSO are sequentially added into the production waste water for mixing up pH value under stirring4, then add H2O2Carry out oxygen
Change reaction；Activated carbon dosage is 0.5~2g/L；
(3) alkali is added to adjust its pH to 9~10 into the production waste water after oxidation；
(4) Al is added into the processed production waste water of step (3) under stirring2(SO4)3Solution, until reaction system pH to 6~
7, sufficient standing settles to obtain turbid, and filtrate is obtained by filtration to the turbid；
(5) if the filtrate that step (4) obtains reaches COD≤200mg/L, the processing requirement of coloration≤16 times is then concentrated by evaporation, does
Technical grade sulfuric acid sodium is obtained after dry；If the filtrate that step (4) obtains is not up to processing requirement, repeatedly step (2)~(4), directly
To reaching processing requirement；
In step (1) and (3), alkali used is solid sodium carbonate or one kind in 25~35% sodium hydrate aqueous solutions or two
Kind；
In step (2), the solid FeSO that is added4Dosage is 1~10mmol/L, the H being added2O2Mass percentage concentration
For 25~35%, H2O2Dosage is 5~20ml/L.
2. the side of Fenton processing 6- nitro -1,2,4- acid oxysomes production waste water co-production sodium sulphate according to claim 1
Method, which is characterized in that the 6- nitro-1,2,4-sulfonic acids production waste water is 6- nitro-1,2,4-sulfonic acid production processes
In, restore the one or two kinds of composite wastes generated in indexing or acid out step.
3. the side of Fenton processing 6- nitro -1,2,4- acid oxysomes production waste water co-production sodium sulphate according to claim 1
Method, which is characterized in that in step (2), reaction temperature is 25~50 DEG C, and the reaction time is 1~2h, and reactive mode is to stand.
4. the side of Fenton processing 6- nitro -1,2,4- acid oxysomes production waste water co-production sodium sulphate according to claim 1
Method, which is characterized in that in step (4), the Al that is added2(SO4)3Solution quality percent concentration is 10~30%.
5. handling 6- nitro -1,2,4- acid oxysomes according to Claims 1 to 4 any one of them Fenton produces waste water co-production sulphur
The method of sour sodium, which is characterized in that the number for repeating step (2)~(4) is 2~4 times.
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| CN108046403B (en) * | 2017-12-12 | 2021-04-23 | 合肥立方制药股份有限公司 | Treatment method and application of mercapto compound production waste liquid |
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| CN113292416A (en) * | 2021-06-04 | 2021-08-24 | 枣庄市泰瑞精细化工有限公司 | Production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid |
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