CN103803753B - A kind of synthetical recovery treatment process of H acid trade effluent - Google Patents
A kind of synthetical recovery treatment process of H acid trade effluent Download PDFInfo
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- CN103803753B CN103803753B CN201410073751.6A CN201410073751A CN103803753B CN 103803753 B CN103803753 B CN 103803753B CN 201410073751 A CN201410073751 A CN 201410073751A CN 103803753 B CN103803753 B CN 103803753B
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Abstract
The invention discloses the synthetical recovery treatment process of a kind of H acid trade effluent, belong to trade effluent recovery and treatment method field.After the steps include: (1) H acid trade effluent adjust ph to 1.0 ~ 1.5, complexing abstraction is adopted to extract, organism is separated from waste water, extraction water outlet reduces extraction agent through membrane filtration and runs off, extraction agent utilizes 13% sodium hydroxide solution to carry out back extraction, back extraction oil alkali, than 4:1, realizes organic enrichment in the recycling utilization of extraction agent and waste water; (2), after back extraction alkali lye reaches capacity, strip liquor direct reuse, to the alkaline melt workshop section in H acid production, proceeds the production of H acid; (3) regulate pH value to 6 ~ 9 of extraction water outlet, then by MVR technique, concentration and evaporation is carried out to extraction water outlet, reclaim to obtain sodium sulfate.Being combined of abstraction technique of the present invention, membrane separation process and MVR technique can save running cost, and evaporation water outlet COD value reaches chemical industrial park sewage work adapter standard.
Description
Technical field
The invention belongs to trade effluent recovery and treatment method field, more particularly, relate to the synthetical recovery treatment process of a kind of H acid trade effluent.
Background technology
H acid is one of important dyestuff intermediate, produces a large amount of naphthene sulfonic acid systems class waste water in its production process.This COD value of waste water is high, colourity dark, pH=2, belongs to the organic waste water of high density, highly acidity, high salinity and high chroma, can not adopt the method process such as traditional biochemistry and materialization.How will wherein organism and inorganic salt separate, be the difficult point in H acid waste water treatment always.
Treatment process at present for this type of dye intermediate wastewater has absorption method, method of enrichment, carbonization and burning method, membrane separation process, cold method, electrolytic process, chemical oxidization method, has extraction process etc.Absorption method divides charcoal absorption and resin absorption, and charcoal absorption is applicable to the lower wastewater treatment of concentration, and resin absorption utilizes resin absorption organism; Method of enrichment is suitable for processing high density, high salinity organic waste water, and shortcoming is that energy consumption is high; Carbonization and burning method are applicable to the extra high waste water of concentration, but capital intensive, require higher to fuel mass and burn operating conditions; Membrane separation process is simple to operate, but effect is not ideal enough, and fenestra easily blocks; Electrolytic process is applicable to the waste water processing COD0.01 ~ 1g/L, and shortcoming is that power consumption is large, and metal polar plate loss is serious; Chemical oxidization method commonly uses ozone oxidation and H
2o
2oxidation, Ozonation is applicable to the lower waste water treatment of concentration, H
2o
2oxidation style is directly used in the high waste liquid of concentration, during process costly; Extraction process compare be suitable for process toxicity large, concentration is high, the waste water of difficult for biological degradation, select suitable extraction agent, treatment effect is better.So, extraction and chemical treatment can be joined together by the improvement for high density, highly acidity waste water, good regulation effect can be obtained, but abstraction technique can only remove the organism in waste water, inorganic salt a large amount of in waste water are still still deposited, and chemical industrial park enterprise wastewater all enters the adapter of garden sewage work at present, high-salt wastewater can not enter the treatment system of garden sewage work, directly discharge also can cause the waste of a large amount of inorganic salt simultaneously, therefore, this waste water does not obtain optimum handling method always.
Deng Bing, Wang Xiangyun has inquired into complexing abstraction process naphthene sulfonic acid class waste water in the research of naphthene sulfonic acid class waste water complexometric extraction, COD is still higher in the method extraction water outlet, extracting operation temperature is too high can strengthen extraction agent solubleness in water, not installing membrane separation unit additional makes extraction agent loss quantitative change large, the alkali lye of back extraction simultaneously can not be reused, cause alkali charge excessive too much with strip liquor, add running cost, easily cause secondary pollution, and extract water outlet to need through again processing discharge, the a large amount of sodium sulfate dissolved in extraction water outlet directly discharge, to environment.Chen Jinlong, Zhang Weiming etc. adopt DN-910 Absorptive complex wave resin to realize the separating and recovering of H acid wastewater through organic matter in the purification of H acid producing waste water and the Application way of resource reclaim, adsorb the reuse of water saturation metabisulfite solution to H acid, T acidleach cake washing process.Resin absorption technique complicated operation, needs very professional technician's guarantee adsorption and desorption effect.Current H acid production process does not use saturated sulphuric acid soln to carry out filter cake washing through updating, and the method does not follow the tracks of process further to washing water outlet, and the final treatment process of inorganic salt in H acid waste water is not described.
Summary of the invention
1. technical problem
Higher for the extraction water outlet COD value existed in prior art H acid Industrial Wastewater Treatment, extraction agent loss amount is large, back extraction alkali lye is too much, the problem that high-salt wastewater directly discharges, the invention provides the synthetical recovery treatment process of a kind of H acid trade effluent, the method can realize water outlet COD value and reach chemical industrial park sewage work adapter standard, extraction agent loss amount is lower than 5/10000ths (extract 10000 tons of waste water and lose 5 tons of extraction agents), useless Organic substance in water is back to use in production, and by MVR process by-product Sodium sulfate anhydrous.min(99) (Disodium sulfate decahydrate), realize the complete qualified discharge of waste water.
2. technical scheme
A synthetical recovery treatment process for H acid trade effluent, the steps include:
(1) behind H acid trade effluent adjust ph to 1.0 ~ 1.5, complexing abstraction is adopted to extract, organism is separated from waste water, extraction water outlet reduces extraction agent through membrane filtration and runs off, extraction agent utilizes 13%(mass ratio) sodium hydroxide solution carries out back extraction, back extraction oil alkali is than 4:1(volume ratio), realize organic enrichment in the recycling utilization of extraction agent and waste water;
This is that organism is transferred in extraction agent due to how sulphonic acids generation complex reaction in acidic conditions extraction agent and H acid waste water, when waste water ph is that effect of extracting is best between 1.0 ~ 1.5; After extraction agent adds liquid caustic soda, pH value becomes alkalescence, in extraction agent and H acid waste water, how sulphonic acids generation decomplexing reacts, organism is transferred in strip liquor again, adopt the sodium hydroxide solution (mass ratio) of 13% as strip liquor, back extraction oil alkali, than 4:1, can ensure that strip liquor is reused 20 times and reached capacity later; Extraction water outlet can realize extraction agent and effectively be separated with extraction water outlet after ultrafiltration membrance filter, makes extraction agent turnover rate control within 5/10000ths;
(2), after back extraction alkali lye reaches capacity, strip liquor direct reuse, to the alkaline melt workshop section in H acid production, proceeds the production of H acid;
(3) regulate pH value to 6 ~ 9 of extraction water outlet, then by MVR technique, concentration and evaporation is carried out to extraction water outlet, reclaim and obtain sodium sulfate.
Extraction water outlet is limpid bright, there are a large amount of inorganic salt, still do not meet chemical industrial park adapter standard, and cause the waste of a large amount of inorganic salt, by MVR technique, concentration and evaporation is carried out to extraction water outlet after adjust ph, recovery obtains sodium sulfate can as selling acquisition economic worth outside by-product, and evaporation water outlet reaches garden adapter standard and can directly discharge.
MVR re-uses its self energy of secondary steam of producing, thus reduces a power-saving technology of the demand of the energy to external world, at present because it is energy-efficiently widely used in solid-liquid separation process.
Preferably, the H acid trade effluent adjust ph acid used in described step (1) is industrial sulphuric acid.
Preferably, the extraction process service temperature in described step (1) is 30 ~ 40 DEG C.
Preferably, the extraction agent in described step (1) is that trialkyl tertiary amine and sulfonated kerosene mix according to mass ratio 1:2.
Preferably, the membrane separation process in described step (1) adopts ultrafiltration membrance filter, and operational condition is temperature 25 ~ 35 DEG C, pressure 0.3 ~ 0.5MPa.
Preferably, described H acid trade effluent is the H acid mother liquor that the finishing operation segregation workshop section of H acid production process produces, and H acid content is at more than 3000mg/L.
Preferably, in described step (3), MVR technique is continuous operation, and evaporation concentration is than the volume ratio for 1:1 ~ 2:3(distillation amount and vinasse).
In H acid producing waste water, sodium sulfate realizes resource utilization and reclaims after " extraction+membrane sepn+MVR " process, and in H acid producing waste water, organism realizes resource utilization recovery after " extraction+back extraction concentrated+reuse to alkaline melt workshop section " processes.
3. beneficial effect
Compared to prior art, the invention has the advantages that:
(1) extraction process utilizes the extraction agent and the waste water that are insoluble in water, makes sulfonic acid substance and extraction agent in waste water carry out the combination of physics or chemistry, realize organic phase transition, then by regulating the chemical property of extraction agent, realize organic transfer enrichment.MVR is the abbreviation of mechanical vapor recompression technology (mechanicalvaporrecompression).Mvr is the energy re-using the secondary steam that it self produces, thus reduces a power-saving technology of the demand of the energy to external world.The present invention adopts extraction and MVR combination process to realize the resource utilization of H acid waste water; The present invention can be applied to during the industry of H acid producing waste water amplifies preferably, is a kind ofly meet the very strong novel process of industrialization demand, practicality;
(2) the present invention employing is as aminated compounds extraction agent (trialkyl tertiary amine and sulfonated kerosene mix according to mass ratio 1:2), H acid waste water is extracted, the organism realized in waste water is separated with water, carry out back extraction by alkali lye again to realize organism and be separated with extraction agent, extraction agent recycle.Saturated strip liquor is back to use the alkaline melt workshop section in production, realizes the recovery of H acid, make the organism in waste water be recycled utilization, reduce organic discharge to greatest extent, realize resource utilization;
(3) present invention achieves extraction water outlet organic content low, containing a large amount of sodium sulfate in water outlet, after evaporation concentration, the sodium sulfate of technical grade of purifying out can beyond sell, for enterprise bring economic interests while realize discharged wastewater met the national standard;
(4) the extracting process easy handling that the present invention relates to, adopt membrane separation technique to reduce extraction agent loss to greatest extent and saved running cost, evaporation concentration adopts MVR technology, and capacity usage ratio is high, runs simple-to-maintain convenient;
(5) the present invention is simple to operate, running cost is low, energy consumption is low, and the H acid of recovery, Sodium sulfate anhydrous.min(99) can be sold and be brought economic interests, reduces scale wastewater treatment burden.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of embodiment 1.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, technical scheme of the present invention is described further.
Embodiment 1
As shown in arrow points in Fig. 1, extraction agent is stored in solvent tank 1, H acid producing waste water is stored in waste water tank, waste water tank is with heating function, during operation, H acid wastewater temperature can be remained on 30 ~ 40 DEG C by waste water tank, waste water and extraction agent are promoted in static mixer 1 by volume pump, gun barrel 1 is entered wherein after waste water fully mixes with extraction agent, during continuous operation, extraction agent is from flowing in solvent tank 2, extraction water outlet enters membrane separation unit, after membrane sepn, water outlet enters wastewater disposal basin, extraction agent after membrane sepn enters solvent tank 2, alkali lye in extraction agent in solvent tank 2 and reextraction flow container is promoted in static mixer 2 through volume pump, after abundant mixing, mixed solution enters in gun barrel 2, after layering, extraction agent flows in solvent tank 1 and continues to use, saturated strip liquor enters in saturated back extraction flow container, then alkaline melt workshop section in reuse to H acid production, continue the production of H acid.Regulate extraction water outlet pH value to 6 ~ 9 stored in wastewater disposal basin, pump in MVR vaporizer through lift pump, after evaporative crystallization, water outlet enters official website, garden, and by-product is sodium sulfate.
The H acid waste water of this example to certain printing and dyeing mill processes, and this waste water quality is in Table 1-1.
Table 1-1
| Project | pH | COD（mg/L） | H acid content (mg/L) | Total salt quantity (mg/L) |
| H acid waste water | 2～3 | 22000 | 3900 | 310000 |
This H acid producing waste water is stored in the waste water tank of 5t, volume pump pumps into 50% industrial sulphuric acid solution wherein, through the automatic adjust ph to 1.0 of online pH meter, water temperature in waste water tank is remained on 30 DEG C by heating system, 1t trialkyl tertiary amine and 2t sulfonated kerosene are added in 5t solvent tank 1, solution pump in waste water tank and solvent tank 1 enters in static mixer 1 with 4L/min by two volume pumps, enter in gun barrel 1 after in mixing 5min, after being separated, extraction agent enters in solvent tank 1, extracting water temp is 28 DEG C, (employing ultra-filtration membrane) in membrane separation unit is pumped into through pump, pressure reaches 0.4MPa, after membrane sepn, water outlet enters wastewater disposal basin, isolated extraction agent enters in solvent tank 2, by massfraction be 13% liquid caustic soda add in 5t back extraction flow container, in solvent tank 2, the liquid caustic soda of extraction agent and back extraction flow container pumps into 4L/min and 1L/min in static mixer 2 respectively through volume pump, enter in gun barrel 2 after mixing 5min, after layering, extraction agent flows in solvent tank 1 and continues to use, back extraction alkali lye enters saturated back extraction flow container kind, enters H acid and produce alkaline melt workshop section continuation H acid production after having stored.Extraction water outlet enters in wastewater disposal basin after membrane filtration, enters MVR multi-effect evaporation system, passes into steam and starts evaporation, and evaporation concentration is than being 1:1, and waste water obtains by-product sodium sulfate crystal after MVR multiple-effect evaporation is concentrated, and water outlet enters garden pipe network.Evaporation concentration effluent quality is in Table 1-2.
Table 1-2
| Project | pH | COD（mg/L） | H acid content (mg/L) | Total salt quantity (mg/L) |
| Distillation water outlet | 7.5 | 280 | — | 570 |
Known after extraction, MVR multiple-effect evaporation concentrate by table 1-2, water outlet reaches chemical industrial park sewage work adapter standard completely.Adapter standard in chemical industrial park is in Table 1-3.
Table 1-3
| Sequence number | Project | Sewage adapter standard |
| 1 | pH | 6-9 |
| 2 | COD | ≤500/L |
| 3 | Salinity | ≤5000mg/l |
After MVR multiple-effect evaporation concentrates, the Sodium sulfate anhydrous.min(99) of system can reach the standard of acceptable end product completely.Table 1-4 is the quality and technical index of Sodium sulfate anhydrous.min(99):
Table 1-4
Embodiment 2
The H acid waste water of the present embodiment to certain printworks processes, and this waste water quality is in Table 2-1.
Table 2-1
| Project | pH | COD（mg/L） | H acid content (mg/L) | Total salt quantity (mg/L) |
| H acid waste water | 2～3 | 20000 | 4000 | 330000 |
(1) extract
Get the H acid waste water of 500mL, add 0.5mL industrial sulphuric acid and pH value is adjusted to 1.5, heating in water bath to 40 DEG C, adds 500mL extraction agent, by waste water and extraction agent Homogeneous phase mixing, after oscillation extraction 5min, stratification 5min, lower floor extracts water temp and is reduced to 34 DEG C, and extraction water outlet retains extracting and enriching agent after ultra-filtration membrane filters under 0.5MPa, then be transferred in 1000mL distilling flask by extraction water outlet, lower floor's extraction agent is retained in separating funnel.Extraction effluent quality is in Table 2-2:
Table 2-2
| Project | pH | COD（mg/L） | H acid content (mg/L) | Total salt quantity (mg/L) |
| Extraction water outlet | 3 | 300 | 12 | 330000 |
(2) back extraction
Be the sodium hydroxide solution of 13% by the mass concentration configured, heating in water bath is to 35 DEG C, join in separating funnel and back extraction is carried out to extraction agent, oil alkali than 4:1, after oscillation extraction 5min, stratification 20min, after layering, extraction agent continues to use, alkali lye proceeds back extraction, gets back to alkaline melt workshop section in production after alkali lye back extraction 20 times, reclaims H acid product.
(3) evaporation concentration and Sodium sulfate anhydrous.min(99) are produced
In test, above-mentioned 500mL is extracted water outlet and add 0.4g sodium hydroxide adjustment pH to 7.5, flask is placed in heating jacket, connect water distilling apparatus, evaporation concentration under the condition stirred, after distilling out 150mL liquid (distillation effluent quality is in Table 2-3), raffinate is transferred in 3 100mL furnace potes while hot, furnace pot is placed in moisture eliminator, 105 DEG C of dry 4h, obtain content Sodium sulfate anhydrous.min(99) (Sodium sulfate anhydrous.min(99) specific targets are in Table 1-4) more than 95.0%.
Table 2-3
| Project | pH | COD（mg/L） | H acid content (mg/L) | Total salt quantity (mg/L) |
| Distillation water outlet | 7.3 | 180 | — | 430 |
"-" represents lower than detection limit, and known after extraction, evaporation concentration by table 2-3, water outlet reaches chemical industrial park sewage work adapter standard completely.Adapter standard in chemical industrial park is in Table 1-3.
The Sodium sulfate anhydrous.min(99) that present method is produced can reach the standard of acceptable end product completely.Sodium sulfate anhydrous.min(99) technology quality index is in Table 1-4.
Claims (2)
1. a synthetical recovery treatment process for H acid trade effluent, the steps include:
(1) behind H acid trade effluent adjust ph to 1.0 ~ 1.5, complexing abstraction is adopted to extract, organism is separated from waste water, extraction water outlet reduces extraction agent through membrane filtration and runs off, extraction agent utilizes 13% sodium hydroxide solution to carry out back extraction, back extraction oil alkali, than 4:1, realizes organic enrichment in the recycling utilization of extraction agent and waste water;
(2), after back extraction alkali lye reaches capacity, back extraction alkali lye direct reuse, to the alkaline melt workshop section in H acid production, proceeds the production of H acid;
(3) regulate pH value to 6 ~ 9 of extraction water outlet, then by MVR technique, concentration and evaporation is carried out to extraction water outlet, reclaim and obtain sodium sulfate;
Wherein, the H acid trade effluent adjust ph acid used in described step (1) is industrial sulphuric acid;
Wherein, the extraction process service temperature in described step (1) is 30 ~ 40 DEG C;
Wherein, the membrane filtration in described step (1) adopts ultrafiltration membrance filter, and operational condition is temperature 25 ~ 35 DEG C, pressure 0.3 ~ 0.5MPa;
Wherein, described H acid trade effluent is the H acid mother liquor that the finishing operation segregation workshop section of H acid production process produces, and H acid content is at more than 3000mg/L;
Wherein, the extraction agent in described step (1) is that trialkyl tertiary amine and sulfonated kerosene mix according to mass ratio 1:2.
2. the synthetical recovery treatment process of a kind of H acid trade effluent according to claim 1, it is characterized in that, in described step (3), MVR technique is continuous operation, and evaporation concentration is than being 1:1 ~ 2:3.
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| CN109748830A (en) * | 2019-01-09 | 2019-05-14 | 江苏吉华化工有限公司 | A kind of processing solution and processing method for H acid mother liquor |
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