CN104671537B - The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 - Google Patents

The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 Download PDF

Info

Publication number
CN104671537B
CN104671537B CN201510058539.7A CN201510058539A CN104671537B CN 104671537 B CN104671537 B CN 104671537B CN 201510058539 A CN201510058539 A CN 201510058539A CN 104671537 B CN104671537 B CN 104671537B
Authority
CN
China
Prior art keywords
waste water
nitrification
disperse blue
water
mother liquor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510058539.7A
Other languages
Chinese (zh)
Other versions
CN104671537A (en
Inventor
郑鑫
张云保
陈磊
张静
毛兵
杨迪迪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Qicai Eco Technology Co Ltd
Original Assignee
Zhejiang Qicai Eco Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Qicai Eco Technology Co Ltd filed Critical Zhejiang Qicai Eco Technology Co Ltd
Priority to CN201510058539.7A priority Critical patent/CN104671537B/en
Publication of CN104671537A publication Critical patent/CN104671537A/en
Application granted granted Critical
Publication of CN104671537B publication Critical patent/CN104671537B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Water Treatment By Sorption (AREA)

Abstract

The present invention discloses the processing method of nitrification refinement mother liquor waste water of a kind of Disperse Blue-56, comprises the steps: (1) complexometric extraction: waste water is the most acid with the mixed system regulation of extractant, carries out complexometric extraction, isolated aqueous phase I and oil phase I;(2) absorption: aqueous phase I obtains filtrate after carrying out two-stage adsorption filtration: (a) primary adsorption uses adsorbent;B () secondary absorption uses resin adsorption;(3) electrodialysis: filtrate carries out electrodialysis process, obtains dense water and fresh water.The present invention is the process technique served as theme with " extraction-absorption-concentrate ", separates the organic matter of residual in waste water, the COD removed in waste water, colourity step by step, targetedly, obtains cleaner sodium salt solution after concentration.

Description

The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56
Technical field
The present invention relates to Treating Industrial Wastewater field, be specifically related to a kind of nitrification essence of Disperse Blue-56 The processing method of mother liquor waste water processed.
Background technology
Disperse Blue-56 also known as Disperse Blue 2BLN or 1,5-dihydroxy-4,8-diamino-anthraquinone bromide with 1,8-dihydroxy-4, the mixture of 8-diamino-anthraquinone bromide, is a kind of important disperse dyes.Main The dyeing of terylene to be used for and blend fabric, polyamide fibre, poly-vinegar fiber etc. is it can also be used to superfine fibre Dyeing, be one of three primary colors.
The production technology of Disperse Blue-56 mainly has mercury method and non-mercury method two kinds, and wherein, mercury method is due to dirt Dye is serious, has stopped using.After repeatedly improving, using wide technique at present is non-mercury method Phenoxy group method.Conventional flow process is nitrification-phenoxylation-second nitrification-hydrolysis-reduction-bromination.Produce During produce waste water about 14 strands, can apply mechanically for 5 strands, 9 strands must process.Although non-mercury method is compared Mercury method is polluted little, and technique is also being updated, but still produces a large amount of three wastes in its production process. The waste water produced when producing Disperse Blue-56 has high chroma, high soda acid, high COD, low B/C value etc. Feature, therefore this wastewater toxicity is big, biodegradability is poor, it is difficult to subsequent treatment, if do not carried out effectively Environment can be done great damage by improvement.
In existing research, ClO2(bibliography: Zhao Maojun, ClO2To reactive brilliant red k-2g and point Dissipate the decolouring research of blue 2BLN dyestuff, Sichuan environment, volume 20 01 phase calendar year 2001;Xie Jiali, point Dissipate the Chlorine Dioxide Oxidation decolouring research of blue 2BLN dyestuff, phase calendar year 2001 13 volume 02) and ozone (ginseng Examine document: Song Shuan, the research of ultrasound-enhanced ozone oxidation dispersed blue dye waste water, Zhejiang Polytechnical University Journal, 03 phase in 2006) and microorganism (bibliography: Gao Qianqian, plant vector immobilization The research of fungal laccase decolored degradation Disperse Blue 2BLN, Jiangsu's agriculture science, the 3rd phase in 2009) All Disperse Blue-56 waste water there is good decolorizing effect.But, several method is at conceptual phase, Only the Dyestuff synthesis waste water of low concentration there is is decolorizing effect, to the clearance of COD below 50%, Poor effect.
In Disperse Blue-56 production process, the nitro compounds purity after a nitrification is the highest, follow-up for improving Products collection efficiency, refines this nitro compounds.Method be in the product after a nitrification add water, NaOH and sodium sulfite are neutralized refined, create one waste water in subtractive process, and this gives up Containing nitroanthraquinone sulfonic acid sodium salt, nitrous acid sodium salt and sodium sulphate etc. in water, in existing document patent also There is no the open processing method individually processing this strand of waste water.
Summary of the invention
For the showing of processing method the most individually processing nitrification refinement mother liquor waste water of Disperse Blue-56 Shape, the invention discloses the processing method of this waste water a kind of.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 of the present invention, is with " extraction-absorption -concentrate " the process technique served as theme, in a nitrification subtractive process of Disperse Blue-56 production technology Produce the character of waste water, separate the organic matter of residual in waste water step by step, targetedly, remove and give up COD in water, colourity, obtain cleaner sodium salt solution, the letter of present invention process flow process after concentration Single, reaction condition gentleness, easy and simple to handle, effect is obvious.
The processing method of nitrification refinement mother liquor waste water of a kind of Disperse Blue-56, comprises the steps:
(1) complexometric extraction: waste water is the most acid with the mixed system regulation of extractant, is complexed Extraction, isolated aqueous phase I and oil phase I;
(2) absorption: aqueous phase I obtains filtrate after carrying out two-stage adsorption filtration:
A () primary adsorption uses adsorbent;
B () secondary absorption uses resin adsorption;
(3) electrodialysis: filtrate carries out electrodialysis process, obtains dense water and fresh water.
Dense water is used for preparing dyestuff, chemical industry or medicine intermediate, and fresh water is used as fresh water (FW), wash water.Point The waste water of the nitrification process for refining section generation dissipating blue 56 production processes is alkalescence, with the matter of waste water Gauge, wherein contains the natrium nitrosum of about 1.2%, the sodium sulfite of about 0.1% and about 0.02% sulfuric acid Sodium, additionally, waste water has remained part Anthraquinones raw materials for production and product, the dark red blackout of color.Anthracene Quinones organic matter contains sulfonic group, and conventional efficient treating method is complexometric extraction, but this kind of extraction of routine Take and sulfuric acid can only be used to extract.
The production of dyestuff intermediate and wastewater treatment process, often with SO2Or NOxThe generation of gas. As preferably, described NOxGas from the nitration reaction of Disperse Blue-56 or is condensed from Disperse Blue-56 Waste water is removing the process of potassium nitrite.Additionally SO2Can come from H acid, T acid, K acid or 2- The sulfonation process of naphthols etc..These gases are discharged in air and can produce acid rain, endanger Environmental Health, Must reclaim.
For Appropriate application waste gas SO2Or NOx, it is ensured that the effect of complexometric extraction, described step (1) In, in the waste water mixed system with extractant, blast SO2Or NOxRegulation system pH, controls SO2 Or NOxThe amount of blasting, keep waste water pH be adjusted to 1-3.5;
These waste gas are effectively utilized by the present invention, use SO2Or NOxGas is to Disperse Blue-56 once Nitrification refinement mother liquor aerating wastewater, regulates its pH, carries out complexometric extraction.It is passed through SO2Or NOxGas When body to extraction system is acidity, the Organic Sodium Salt in waste water is converted into inorganic sodium, mainly with nitrous Acid sodium-salt or sodium sulfate salt are main, further raising natrium nitrosum or the content of sodium sulfate salt, final To sodium-salt aqueous solution, then it is back to use in other production processes, improves the surcharge that waste water processes.
The present invention also can be with the pH of conventional means regulation waste water with the mixed system of extractant, to carry out Complexometric extraction, in described step (1), adds mass fraction in the waste water mixed system with extractant For sulfuric acid or nitric acid regulation system pH that mass fraction is 10-65% of 10-98%, keep waste water PH is adjusted to 1-3.5.
In described step (1), extractant is the mixed solution of tertiary amine and diluent, tertiary amine and dilution The volume ratio of agent is 1: 1-5;Extractant is 3: 0.5-4 with wastewater volume ratio.
Preferably, described tertiary amine is trioctylamine or trialkylamine, and diluent is sulfonated kerosene, two chloroethenes One in alkane, toluene, n-hexane, dimethylbenzene.
As preferably, described tertiary amine is trioctylamine, and diluent is sulfonated kerosene;Wherein trioctylamine and sulphur Changing kerosene volume ratio is 1: 1.5-2.5, and extractant is 3: 0.5-1.5 with wastewater volume ratio.
It has been investigated that, the aqueous phase I after complexometric extraction close to clarification, COD clearance more than 80%, Be conducive to the carrying out of subsequent reactions.
Although the water outlet of complexometric extraction (aqueous phase I) water quality is preferable, but still containing trace oiliness thing, need Carry out primary adsorption, use the trace oiliness thing in adsorbent aqueous phase I.As preferably, described In step (a), adsorbent be activated carbon powder, activated carbon glue, bentonite, diatomite, molecular sieve, At least one in aluminum oxide;The 0.01-2% adding the quality that quality is aqueous phase I of adsorbent.Stir Filter after mixing 0.1-1h and separate.
The microextraction agent of residual when the purpose of addition adsorbent is sorption extraction, and remove mother further The COD of liquid and colourity, prevent the extractant contamination and plugging polymeric adsorbent of residual in aqueous phase, impact tree Fat adsorption effect and parsing.
In order to make full use of extractant, extractant need to be carried out back extraction and be recycled, described step (1) liquid caustic soda that oil phase I mass fraction is 8%-13% obtained regulates its pH to 8.5-10, 40-60 DEG C of insulated and stirred back extraction 0.5-2 hour.
Back extraction terminates rear solution left standstill and separates, and the oil phase II obtained continues to do extractant, and reuse is to step (1) in;The back extraction alkali lye circulation obtained is used as back washing agent.
Back extraction alkali lye is recycled as back washing agent, until when the viscosity increase of back extraction alkali lye, pH < 8, right Back extraction alkali lye focuses on.
In view of reality application and two factors of cost, selecting mass body fraction is the hydrogen-oxygen of 8-13% Change sodium solution preferable as back washing agent.When concentration of sodium hydroxide solution is bigger, aqueous phase poor fluidity, no It is beneficial to transfer and burns;When concentration of sodium hydroxide solution is less, required back extraction alkali lye amount is big, produces dirt Water is many, is also unfavorable for burning, and the cost of burning is also greatly improved.
For removing the COD in aqueous phase I and colourity further, in described step (b), divide by quality After the sodium hydrate aqueous solution regulation primary adsorption that number is 5-48%, the pH to 6-7 of aqueous phase I, crosses macropore Resin adsorption, aqueous phase I is not more than 180 with the volume ratio of resin.
COD≤the 5mg/L of secondary absorption water outlet.Consider resin adsorption conditions, elute, load, The factors such as price, (Xi'an vast space resin science and technology is limited for final selection HYA-106 macroporous absorbent resin Company) as polymeric adsorbent.HYA-106 macroporous absorbent resin has the advantage that one is adsorption bar Part meets the condition of aqueous phase after Absorptive complex wave;Two is that adsorbance is big, adsorbable 180 times of resin volumes filter Liquid just reaches saturated;Three is to resolve easily, and the mass fraction that only need to use 3 times of resin volumes is 4% Sodium hydrate aqueous solution wash-out, can resolve completely.
Use electrodialysis that secondary absorption water outlet is concentrated, obtain dense water and fresh water.
After resin adsorption, the salt content of aqueous phase improves to 8% (in terms of the quality of aqueous phase after resin adsorption) Left and right, carries out electrodialysis to the mother liquor after resin adsorption, and its salt of concentrate assigns to 15% (with dense water quality Meter).Dense water for obtaining electrodialysis is used, and improves the surcharge that waste water processes, described In step (3), reinforcing body sodium salt in dense water, with dense water quality gauge, make the sodium salt content of dense water It is 30%, in other technical process;Or, in described step (3), dense water is concentrated system Salt is to reclaim sodium sulphate or sodium nitrate.
According to the pH of waste gas regulation mixed system in step (1), the gas blasted is different, finally The main component obtaining dense water is different, and dense water can be back to different technical process.Use NOxAeration, Dense water is used for preparing diazo reagent, participates in the synthesis of azo dyes, and the dense water now obtained is nitrous acid Sodium-salt aqueous solution, can be used for the diazo-reaction of azo dyes, as Red 167, disperse blue 183, the diazo-reaction of the dyestuff such as disperse yellow 3, it is to avoid use high energy consumption evaporates unpurified salt, Reduce energy consumption to pollute;Or, use SO2Aeration, dense water is for the essence of itrated compound of Disperse Blue-56 System.The dense water now obtained is sulfite solution.
The isolated fresh water of electrodialysis can be used for washings or the process water of Chemical Manufacture.
Present invention have the advantage that complexation extraction can absorb in other reactions steps and produce Nitrous oxides exhaust gas and oxysulfide waste gas, sodium nitrite in aqueous solution or the sodium sulfite of generation are water-soluble Liquid can be used for diazo-reaction or reduction reaction;Whole technical process does not produce waste gas, and method safety is high Effect, saves the processing cost of waste water and gas, improves its surcharge processed.
Accompanying drawing explanation
Fig. 1 is the process flow figure of nitrification refinement mother liquor waste water of Disperse Blue-56 of the present invention.
Detailed description of the invention
Embodiment 1
Nitrification refinement mother liquor waste water of Disperse Blue-56 after preliminary filtration, record pH be 11.42, COD is about 275000mg/L, in terms of the quality of waste water, containing natrium nitrosum 1.2%, sodium sulfite 0.1%, sodium sulphate 0.02%.
(1) complexometric extraction: by 300mL extractant extractant is trioctylamine: sulfonated kerosene=1: 2 (volume ratios) } stir with 100mL waste water, it is passed through nitrogen oxides NOxIts pH of gas regulation To 3, aerated reaction stands 0.5 little layered after 1 hour, separate oil phase I and aqueous phase I.
It is dark red black that reaction terminates rear oil phase I color, and aqueous phase I is red, transparent supernatant liquid.Water The COD=1600mg/L of phase I, in terms of the quality of aqueous phase I, the content of natrium nitrosum is 7%, nitre The content of acid sodium is 0.1%, and the content of sodium sulphate is 0.03%.
(2) back extraction: the oil phase I after complexometric extraction is added the NaOH that mass fraction is 10% The aqueous solution regulates its pH to 10, stratification after 45 DEG C of lower stirrings of insulation are reacted 0.5 hour, point Go out to separate oil phase II and aqueous phase II.
Reaction terminates rear oil phase II lighter, shows slightly red;Aqueous phase II understands through detection, contains Organic matter, salinity, moisture and NaOH.
(3) primary adsorption: add 0.1g activated carbon in 100g aqueous phase I, stir 0.5 hour Filter, separate, filtrate achromaticity and clarification.
After testing, the COD of this filtrate is 1027.5mg/L.
(4) secondary absorption: the filtrate obtained by primary adsorption is passed through HYA-106 macroporous absorbent resin The chromatographic column that (Xi'an Han Yu resin Science and Technology Ltd.) fills, is the hydrogen-oxygen of 30% with mass fraction Change sodium water solution and regulate its pH to 7.
After testing, the COD=5mg/L of secondary absorption water outlet.
(5) electrodialysis: secondary absorption water outlet carries out electrodialysis process, the salt content detecting dense water is Time 15% (with dense water quality gauge), stop electrodialysis, obtain dense water and fresh water.
After testing, the COD < 5mg/L of fresh water, for colourless transparent liquid, dense water is water white transparency liquid Body.
Comparative example 1
Keep other condition in embodiment 1 constant, remove activated carbon primary adsorption step, directly enter Row secondary absorption, finds that in adsorption process, resin gradually dyes, and causes resin to block, and secondary absorption goes out The COD=475.3mg/L of water.After electrodialysis, fresh water COD > 5mg/L, it is impossible to meet industry Watering condition;Fortified aqueous is coloured, is unsuitable for the synthesis material of other dyestuffs, in order to avoid polluted product, Affect coloured light.
Comparative example 2
Keeping other condition in embodiment 1 constant, secondary absorption step uses D201 type ion to hand over Change resin (Xi'an Han Yu resin Science and Technology Ltd.) absorption, secondary absorption water outlet COD=5mg/L. When resin resolves, use the sodium hydrate aqueous solution that mass fraction is 4% of 6 times of resin volumes, tree Fat is resolved the most completely.After electrodialysis, fresh water COD=5mg/L, water white transparency, dense water is nothing Look transparent mass fraction is the salting liquid of 15%.
From comparative example 2: the effect using D201 type ion exchange resin is big with HYA-106 Macroporous adsorbent resin is identical, but it is 4% that D201 type ion exchange resin resolves used mass fraction Sodium hydrate aqueous solution be the twice of HYA-106 macroporous absorbent resin.
Comparative example 3
Keeping other condition in embodiment 1 constant, back extraction uses mass fraction to be the hydrogen of 30% Aqueous solution of sodium oxide, during stratification, system presents three layers, and lower floor is black mucus, and intermediate layer is Canescence particulate material, upper strata is limpider extractant.After testing, the loss of upper strata extractant Rate is more than 10%.
From comparative example 3: during the excessive concentration of back washing agent, back extraction poor effect, extractant loses Amount is big.
Comparative example 4
Keeping other condition in embodiment 1 constant, back extraction uses mass fraction to be the hydrogen-oxygen of 4% Changing sodium water solution, oil phase is obvious with aqueous phase layering, but aqueous phase is sufficiently bulky, expends NaOH water Solution is a lot, and produced sewage quantity is the biggest.During sodium hydroxide solution just becomes after recycling 2 times Property, become waste liquid.After testing, in waste liquid, solid content is less than 6%, reclaims the most organic cost The highest, the cost of burning disposal is very the biggest.
Embodiment 2
Nitrification refinement mother liquor waste water of Disperse Blue-56 after preliminary filtration, record pH be 11.3, COD is about 279050mg/L, in terms of the quality of waste water, containing natrium nitrosum 1.2%, sodium sulfite 0.1%, sodium sulphate 0.02%.
(1) complexometric extraction: { extractant is trioctylamine: sulfonated kerosene=1: 2 by 300mL extractant (volume ratio) } stir with 100mL waste water, it is passed through SO2Gas regulation its pH to 2.5, room Temperature reaction stood 0.5 hour after 1 hour, and layering obtains oil phase I and aqueous phase I.
It is dark red black that reaction terminates rear oil phase I color, and aqueous phase I is the transparent supernatant liquid of blush. The COD=603mg/L of aqueous phase I, in terms of the quality of aqueous phase I, content of sodium nitrite is 7%, nitric acid Sodium content is 0.1%, and sodium sulphate content is 0.02%.
(2) back extraction: adding mass fraction in oil phase I after complexometric extraction under 50 DEG C of insulations is The sodium hydrate aqueous solution of 13% regulates its pH to 9, and static layering obtains oil phase II and aqueous phase II.
Reaction terminates rear oil phase II lighter, presents light yellow;Aqueous phase II understands through detection, Containing organic matter, salinity, moisture and a small amount of NaOH.
(3) primary adsorption: add 0.1g diatomite in 100g aqueous phase I, stir 0.5 hour Filter and separate.
Filtrate achromaticity and clarification, after testing, the COD of this filtrate is 475mg/L.
(4) secondary absorption: filtrate is passed through HYA-106 macroporous absorbent resin and fills chromatographic column, go out Water mass fraction be 5% sodium hydrate aqueous solution regulate its pH to 6.
After testing, the COD=5mg/L of secondary absorption water outlet.
(5) electrodialysis: secondary absorption water outlet is carried out electrodialysis process, detecting dense water salt content is Time 15% (in terms of the quality of dense water), stop electrodialysis, obtain dense water and fresh water.
After testing, the COD < 5mg/L of fresh water, for colourless transparent liquid.
Comparative example 5
Keep other condition in embodiment 2 constant, remove electrodialysis step, change high energy into and evaporate Salt.High energy evaporation obtains one-level distilled water, and its COD=5mg/L can be used for Chemical Manufacture.Gained The solid salt arrived after testing, containing sodium sulfite 93.3%, sodium sulphate 5%, natrium nitrosum 1.5%, Sodium nitrate 0.2% (being mass fraction above).
Comparative example 6
Keeping other condition in embodiment 2 constant, extractant uses trioctylamine and dichloroethanes with phase Same proportions, is obtained by extraction the COD=1533mg/L of aqueous phase I.Show: sulfonated kerosene is excellent The diluent of choosing.
Comparative example 7
Keeping other condition in embodiment 2 constant, extractant changes 3: 2 into the volume ratio of waste water, The COD=21787mg/L of aqueous phase I is obtained by extraction, after the method described in embodiment 2 processes, two The COD about 360mg/L of level absorption water outlet, in the sodium sulfite salting liquid being concentrated to give, impurity is higher, Cannot be directly used to Dyestuff synthesis.The aqueous phase obtained after aqueous phase I is carried out reextraction COD=904mg/L, reaches after subsequent treatment to use requirement.
Comparative example 7 shows: when extractant is excessive with the volume ratio of waste water, need to carry out multitple extraction.
Comparative example 8
Keep other condition in embodiment 2 constant, the pH of extraction system is adjusted to 4, extracts To the COD=153907mg/L of aqueous phase I, after the method described in embodiment 2 processes, secondary absorption The COD of water outlet about 10060mg/L 10 times of resin volume (wastewater volume be), is concentrated to give In sodium sulfite salting liquid, impurity is a lot, it is impossible to be directly used in Dyestuff synthesis.Aqueous phase I is carried out secondary The aqueous phase COD=64904mg/L obtained after extraction, still can not reach after subsequent treatment to use requirement.
Comparative example 7 shows: when during extraction, pH is too high, and extraction efficiency is remarkably decreased, and finally processes effect Fruit is the most up to standard.
Embodiment 3
Nitrification refinement mother liquor waste water of Disperse Blue-56 after preliminary filtration, record pH be 11.3, COD is about 279050mg/L, in terms of the quality of waste water, containing natrium nitrosum 0.8%, sodium sulfite 0.1%, sodium sulphate 0.8%.
(1) complexometric extraction: { extractant is trioctylamine: sulfonated kerosene=1: 2 by 300mL extractant (volume ratio) } stir with 100mL waste water, with Disperse Blue-56 second nitrification waste water (sulfur-bearing Acid about 25%) regulate its pH to 2.5, stand 0.5 hour after reaction being stirred at room temperature 0.5 hour, point Layer obtains oil phase I and aqueous phase I.
It is dark red black that reaction terminates rear oil phase I color, and aqueous phase I is the transparent supernatant liquid of blush. The COD=321mg/L of aqueous phase I, in terms of the quality of aqueous phase I, content of sodium nitrite is 0.2%, nitre Acid sodium content is 0.5%, and sodium sulphate content is 2.2%.
(2) back extraction: adding mass fraction in oil phase I after complexometric extraction under 50 DEG C of insulations is The sodium hydrate aqueous solution of 13% regulates its pH to 9, and static layering obtains oil phase II and aqueous phase II.
Reaction terminates rear oil phase II lighter, presents light yellow;Aqueous phase II understands through detection, Containing organic matter, salinity, moisture and a small amount of NaOH.
(3) primary adsorption: add 0.1g diatomite in 100g aqueous phase I, stir 0.5 hour Filter and separate.
Filtrate achromaticity and clarification, after testing, the COD of this filtrate is 188mg/L.
(4) secondary absorption: filtrate is passed through HYA-106 macroporous absorbent resin and fills chromatographic column, go out Water mass fraction be 5% sodium hydrate aqueous solution regulate its pH to 6.
After testing, the COD=5mg/L of secondary absorption water outlet.
(5) electrodialysis: secondary absorption water outlet is carried out electrodialysis process, detecting dense water salt content is Time 15% (in terms of the quality of dense water), stop electrodialysis, obtain dense water and fresh water.
After testing, the COD < 5mg/L of fresh water, for colourless transparent liquid.
(6) condensing crystallizing: obtain sodium sulfate salt by after concentration, meet national standard.

Claims (10)

1. the processing method of nitrification refinement mother liquor waste water of a Disperse Blue-56, it is characterised in that comprise the steps:
(1) complexometric extraction: waste water is the most acid with the mixed system regulation of extractant, carries out complexometric extraction, isolated aqueous phase I and oil phase I;
(2) absorption: aqueous phase I obtains filtrate after carrying out two-stage adsorption filtration:
A () primary adsorption uses adsorbent;
B () secondary absorption uses resin adsorption;
(3) electrodialysis: filtrate carries out electrodialysis process, obtains dense water and fresh water.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 1, it is characterised in that in described step (1), blasts SO in the waste water mixed system with extractant2Or NOxRegulation system pH, controls SO2Or NOxThe amount of blasting, keep waste water pH be adjusted to 1-3.5;
Or, in described step (1), in the waste water mixed system with extractant, add the sulfuric acid that mass fraction is 10-98% or nitric acid regulation system pH that mass fraction is 10-65%, keep the pH of waste water to be adjusted to 1-3.5.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 1, it is characterised in that in described step (1), extractant be the volume ratio of the mixed solution of tertiary amine and diluent, tertiary amine and diluent be 1:1-5;Extractant and wastewater volume are than for 3:0.5-4.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 3, it is characterised in that described tertiary amine is trioctylamine or trialkylamine, diluent is the one in sulfonated kerosene, dichloroethanes, toluene, n-hexane, dimethylbenzene.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 4, it is characterised in that described tertiary amine is trioctylamine, diluent is sulfonated kerosene;Wherein trioctylamine and sulfonated kerosene volume ratio are 1:1.5-2.5, and extractant and wastewater volume ratio is for 3:0.5-1.5.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 1, it is characterized in that, in described step (a), adsorbent is at least one in activated carbon powder, activated carbon glue, bentonite, diatomite, molecular sieve, aluminum oxide;The 0.01-2% adding the quality that quality is aqueous phase I of adsorbent.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 1, it is characterized in that, the liquid caustic soda that oil phase I mass fraction is 8%-13% that described step (1) obtains regulates its pH to 8.5-10,40-60 DEG C of insulated and stirred back extraction 0.5-2 hour
Back extraction terminates rear solution left standstill and separates, and the oil phase II obtained continues to do extractant, in reuse to step (1);The back extraction alkali lye circulation obtained is used as back washing agent.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 1, it is characterized in that, in described step (b), with the pH to 6-7 of aqueous phase I after the sodium hydrate aqueous solution regulation primary adsorption that mass fraction is 5-48%, crossing macroporous absorbent resin absorption, aqueous phase I is not more than 180 with the volume ratio of resin.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 2, it is characterised in that in described step (3), reinforcing body sodium salt in dense water, with dense water quality gauge, the sodium salt content making dense water is 30%;
Or, in described step (3), dense water is concentrated salt manufacturing to reclaim sodium sulphate or sodium nitrate.
The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 the most according to claim 2, it is characterised in that use NOxAeration, dense water is used for preparing diazo reagent, participates in the synthesis of azo dyes;
Or, use SO2Aeration, dense water refining for itrated compound of Disperse Blue-56.
CN201510058539.7A 2015-02-05 2015-02-05 The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56 Active CN104671537B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510058539.7A CN104671537B (en) 2015-02-05 2015-02-05 The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510058539.7A CN104671537B (en) 2015-02-05 2015-02-05 The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56

Publications (2)

Publication Number Publication Date
CN104671537A CN104671537A (en) 2015-06-03
CN104671537B true CN104671537B (en) 2016-08-17

Family

ID=53307199

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510058539.7A Active CN104671537B (en) 2015-02-05 2015-02-05 The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56

Country Status (1)

Country Link
CN (1) CN104671537B (en)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105036428A (en) * 2015-07-27 2015-11-11 南通昊友食品添加剂有限公司 Method for softening treatment of water used for food additives
CN105060558B (en) * 2015-08-04 2017-06-27 浙江闰土研究院有限公司 A kind of pretreatment of Disperse Blue-56 condensation waste water and resource utilization method
CN105923685B (en) * 2016-05-12 2019-04-12 浙江丝科院轻纺材料有限公司 A kind of method that multi-alkylamine extration resin captures dyes in dyeing waste water
CN106044971A (en) * 2016-07-21 2016-10-26 沧州中铁装备制造材料有限公司 High-temperature electrodialysis desalination method for saline
CN109534528B (en) * 2018-11-20 2021-11-12 新昌县泰如科技有限公司 Method for treating ciprofibrate process wastewater
CN113104865B (en) * 2019-12-12 2023-08-22 酒泉宇鹏化工科技有限公司 Treatment method of vat blue RSN refining mother liquor
CN110981063A (en) * 2019-12-19 2020-04-10 天门楚天生物科技有限公司 Comprehensive treatment method of disperse blue 56-benzene oxidation wastewater
CN111115744A (en) * 2020-01-10 2020-05-08 浙江长征化工有限公司 Treatment method of disperse red 60 condensed wastewater
CN111253773A (en) * 2020-02-21 2020-06-09 扬州日兴生物科技股份有限公司 Method for producing disperse blue by using 1-aminoanthraquinone DMF residue
CN111268843B (en) * 2020-02-28 2022-04-22 河北大鹏医药化工有限公司 Process for recovering nitric acid from nitrified wastewater
CN113248069B (en) * 2021-07-05 2021-10-22 北京惠宇乐邦环保科技有限公司 Treatment method of disperse blue 56 production wastewater

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101104533B (en) * 2007-06-05 2011-07-27 南开大学 Method for treating waste water of H-acid production
CN103241885A (en) * 2013-05-15 2013-08-14 绍兴奇彩化工有限公司 Method for treating acid waste water of disperse dye
CN103408092B (en) * 2013-08-02 2015-01-07 浙江吉华集团股份有限公司 Treatment method for production wastewater of sulfonic acid group dye and dye intermediate of sulfonic acid group dye

Also Published As

Publication number Publication date
CN104671537A (en) 2015-06-03

Similar Documents

Publication Publication Date Title
CN104671537B (en) The processing method of nitrification refinement mother liquor waste water of Disperse Blue-56
CN105502779B (en) The processing method of condensation waste water in a kind of Disperse Blue-56 production process
CN105259011B (en) A kind of Soil fulvic acid subfraction fractional extraction method
CN104609618B (en) The treatment process of Disperse Blue-56 mother-liquor waste water
CN103408092B (en) Treatment method for production wastewater of sulfonic acid group dye and dye intermediate of sulfonic acid group dye
CN105084600B (en) A kind of method and its application of efficient process salt-containing organic wastewater
CN105130062B (en) A kind of processing method of anthraquinone waste water
CN110902747B (en) Method for recovering bromine from bromine-containing wastewater generated in production of bromoaniline
CN105060552A (en) Method for treating disperse blue 56 reduction mother liquor wastewater
CN104291425A (en) Special flocculation decolorizing agent for fur oxidation dyeing sewage and preparing method thereof
CN110759545A (en) Treatment method of anthraquinone dye waste acid
CN105983393A (en) Preparation method of fly ash chitosan composite adsorbent for treating printing and dyeing wastewater
CN105174582A (en) Resource treatment process of 1-amino anthraquinone sulfurization reduction wastewater
CN105056899A (en) Adsorbent for treating dye-containing wastewater, and preparation and application thereof
CN105152419B (en) A kind of high concentration is containing acid or the processing method of the organic wastewater containing alkali and its application
CN101519249A (en) Method for treating hydrolyzed waste water and recovering resource in disperse blue production process
CN107512810A (en) Method of wastewater treatment after a kind of nitro-chlorobenzene production
CN104829505B (en) The separation method of anthraquinone sulfonic acid in the spent acid that a kind of anthraquinone and derivant production process thereof produce
Zhang et al. Spectroscopic studies of dye-surfactant interactions with the co-existence of heavy metal ions for foam fractionation
CN104445781A (en) Treatment method for fused ring compound wastewater
CN100415654C (en) Process for purifying and resource recovery using from waste water of producing H cide
CN105540926A (en) Method for cooperatively producing white carbon black and inorganic salt with acid wastewater
Zhang et al. Adsorption of methylene blue and Congo red on bentonite modified with CaCO3
CN102953286A (en) Treating method for pulping black liquor
CN106745444B (en) Treatment method of T acid industrial wastewater

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: 312000 Zhejiang province Shaoxing Shunjiang Road No. 683 building 903 room 9

Applicant after: ZHEJIANG QI CAI ECO TECHNOLOGY Co.,Ltd.

Address before: Shaoxing City, Zhejiang province 312000 smartfortune Di Dang new building 17 floor room 1709

Applicant before: ZHEJIANG QICAI ENVIRONMENTAL PROTECTION SCIENCE AND TECHNOLOGY LTD.

Address after: Shaoxing City, Zhejiang province 312000 smartfortune Di Dang new building 17 floor room 1709

Applicant after: ZHEJIANG QICAI ENVIRONMENTAL PROTECTION SCIENCE AND TECHNOLOGY LTD.

Address before: Shaoxing City, Zhejiang province 312000 smartfortune Di Dang new building 17 floor room 1709

Applicant before: SHAOXING QICAI CHEMICAL TECHNOLOGY CO.,LTD.

COR Change of bibliographic data
C14 Grant of patent or utility model
GR01 Patent grant