CN105110536A - Recycling method for high-salinity wastewater containing sodium chloride and sodium sulfate - Google Patents
Recycling method for high-salinity wastewater containing sodium chloride and sodium sulfate Download PDFInfo
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Abstract
The invention discloses a recycling method for high-salinity wastewater containing sodium chloride and sodium sulfate and belongs to the field of wastewater treatment. The method comprises: filtering wastewater through a nanofiltration membrane; performing evaporative crystallization on filtrate through the nanofiltration membrane to obtain sodium chloride and filtered mother liquor; performing evaporative crystallization on retained liquor which does not pass through the nanofiltration membrane to obtain sodium sulfate and retained mother liquor; mixing the filtered mother liquor with the retained mother liquor to obtain a mixture and adding fluosilicic acid into the mixture; and stirring sufficiently the mixture to obtain sodium fluosilicate by filtering. Filtered acid water is used in pH value adjustment of a system before biochemical treatment.
Description
Technical field
The present invention relates to a kind for the treatment of process of waste water, the recovery and treatment method of the high-salt wastewater of especially a kind of sodium chloride-containing and sodium sulfate, belongs to field of waste water treatment.
Background technology
Have large amount of sewage to discharge in Coal Chemical Industry production process, these sewage, except including organism, also include a large amount of salts.Coal chemical industry sewage is cut down organism through biochemical treatment, through filtration treatment filtering solid matter, is consisted predominantly of sodium sulfate, sodium-chlor and other salts of trace, be usually referred to as high-salt wastewater in remaining waste water.
High-salt wastewater cannot complete process by biochemical method, and materializing strategy process is more complicated, and processing costs is higher, is the difficult waste water that sewage treatment industry is generally acknowledged.If the unprocessed direct discharge of these high-salt wastewaters, then will certainly produce high risks to aqueous bio, Drinking Water and industrial and agricultural production water.Constantly study both at home and abroad the treatment technology of high-salt wastewater, in numerous high-salt wastewater treatment technologies, evaporative desalination method because of its technology maturation, the advantages such as waste water scope is wide, processing speed is fast, energy-conservation can be processed develop at home comparatively fast.Evaporative desalination method makes the part water vapor in high-salt wastewater by the method for heating and remove, and to improve the concentration of solution, separates out create conditions for solute.But, the solid adopting simple evaporative desalination method to separate out is all the mixed salt simultaneously comprising multiple salt, purity is low, cannot industrially reuse, usually directly discard or give the useless processing mechanism of danger to carry out professional treatment with higher price, so not only increase environmental protection pressure, also considerably increase the cost for wastewater treatment of factory.
Industrially, sodium sulfate and these two kinds of salt usage quantitys of sodium-chlor are very large, and a large amount of sodium sulfate in high-salt wastewater, sodium-chlor are all discarded in vain, unfortunately.
Summary of the invention
The technical issues that need to address of the present invention are to provide the recovery and treatment method of the high-salt wastewater of a kind of sodium chloride-containing and sodium sulfate, effective recycling can be carried out to the sodium sulfate in high-salt wastewater and sodium-chlor by the method, greatly reduce environmental protection pressure, save the sour water regulating pH value used simultaneously, save cost for wastewater treatment.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
The recovery and treatment method of the high-salt wastewater of sodium chloride-containing and sodium sulfate, high-salt wastewater containing sodium-chlor and sodium sulfate passes through nanofiltration membrane, filtered liquid through nanofiltration membrane obtains sodium-chlor and filtrated stock through evaporative crystallization, trapped fluid not through nanofiltration membrane obtains sodium sulfate and retain mother liquor through evaporative crystallization, filtrated stock adds silicofluoric acid wherein with retaining after mother liquor mixes, filter to obtain Sodium Silicofluoride after abundant stirring, the sour water after filtration is for the adjustment of system pH value before biochemical treatment.
The further improvement of technical solution of the present invention is that concrete steps are:
A, nanofiltration membrane
High-salt wastewater is pumped into the feeding liquid side of nano-filtration unit, through nanofiltration membrane, high-salt wastewater is divided into through the filtered liquid of nanofiltration membrane with not through the trapped fluid of nanofiltration membrane;
Described filtered liquid enters step B process, and described trapped fluid enters step C process;
B, filtered liquid evaporative crystallization
Sent into by filtered liquid in evaporative crystallizer and carry out evaporation concentration and obtain sodium-chlor and filtrated stock, evaporation concentration temperature is 50 ~ 150 DEG C;
The direct extraction of described sodium chloride crystal, filtrated stock enters step D process;
C, trapped fluid evaporative crystallization
Trapped fluid is sent into evaporative crystallizer and carry out evaporation concentration, evaporation concentration temperature is 50 ~ 150 DEG C, after the solid content of solution reaches 2% ~ 30%, stops evaporation; Under 50 ~ 100 DEG C of conditions, carry out solid-liquid separation, obtain sodium sulfate crystal and retain mother liquor;
The direct extraction of described sodium sulfate crystal, retains mother liquor and enters step D process;
D, chemical precipitation
By filtrated stock with retain after mother liquor fully mixes, pump into chemical precipitation unit, in filtrated stock and the mixed solution retaining mother liquor, add silicofluoric acid, uniform stirring, fully after reaction, carry out filtration and make solid-liquid separation, obtain Sodium Silicofluoride precipitation and sour water;
Described Sodium Silicofluoride is directly extraction after filtration, and the sour water after filtration is for the adjustment of system pH value before biochemical treatment.
The further improvement of technical solution of the present invention is: in described steps A, the operating environment of nanofiltration membrane is: pH=2 ~ 11 of high-salt wastewater, and concentration is about 1wt%, and wastewater temperature is 4 ~ 45 DEG C, and working pressure is 0.5 ~ 1.5MPa;
The mould material of the membrane module of described nano-filtration unit is polymeric amide material, and membrane pore size is less than 2nm.
The further improvement of technical solution of the present invention is: detect high-salt wastewater, filtered liquid, trapped fluid, filtrated stock, the organism retained in mother liquor respectively, when high-salt wastewater, filtered liquid, trapped fluid, filtrated stock, retain organic concentration in mother liquor in any one liquid more than 1000mg/L time, use charcoal absorption to exceed standard the organism in solution or processed the organism exceeded standard in solution by catalyzed oxidation, treat that organic concentration is down to 100 ~ below 300mg/L and is entered next treatment step again.
The further improvement of technical solution of the present invention is: be detected filtrate, trapped fluid, filtrated stock, the organism retained in mother liquor respectively, when filtered liquid, trapped fluid, filtrated stock, the organic concentration retained in mother liquor in any one liquid directly send biochemical wastewater treatment operation back to more than during 1000mg/L.
The further improvement of technical solution of the present invention is: carried out respectively washing and drying treatment by the Sodium Silicofluoride of the sodium sulfate crystal of the sodium chloride crystal of step B extraction, step C extraction, step D filtration gained, make sodium sulfate crystal, sodium chloride crystal and Sodium Silicofluoride reach the quality standard of technical grade sodium sulfate, technical grade sodium-chlor, technical grade Sodium Silicofluoride respectively.
The further improvement of technical solution of the present invention is: described evaporative crystallizer comprises vaporizer and crystallizer, and vaporizer is any one in natural-circulation evaporator, falling-film evaporator, pump feed evaporator.
The further improvement of technical solution of the present invention is: described vaporizer is single-effect evaporator, multiple-effect evaporator, MVR vaporizer or TVR vaporizer.
The further improvement of technical solution of the present invention is: crystallizer is any one in the mutation of Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer and above pattern.
The further improvement of technical solution of the present invention is: described crystallizer is provided with the vertical crystallizer eluriating leg.
Owing to have employed technique scheme, the technical progress that the present invention obtains is:
The invention provides the recovery and treatment method of the high-salt wastewater of a kind of sodium chloride-containing and sodium sulfate, carried out efficient recovery to the sodium-chlor in coal chemical industry high-salt wastewater and sodium sulfate, processing condition simple and stable, is convenient to industrialization promotion.Pass through the inventive method, the highly purified sodium-chlor and sodium sulfate that obtain can be reclaimed, simultaneously at filtrated stock with retain in mother liquor and add silicofluoric acid and obtain Sodium Silicofluoride and sour water, sodium-chlor, sodium sulfate and Sodium Silicofluoride meet the specification of quality of technical grade product, can directly recovery or as byproduct sell, not only reach process high-salt wastewater object, meet current Environmental Protection Situation needs, and turn waste into wealth, achieve the recycling of salt, improve the income of factory; Need to send biochemical wastewater treatment operation back to when high-salt wastewater, filtered liquid, trapped fluid, filtrated stock, the organic concentration retained in mother liquor in any one liquid exceed standard, and before biochemical treatment operation, need acid adding to carry out the pH value of regulation system, therefore the sour water produced can be directly used in the pH value regulating system before biochemical treatment, before save the consumption of the acid needed for adjustment of system pH value before biochemical treatment, reduce the processing cost of high-salt wastewater.
The inventive method is a kind for the treatment of process of iterative cycles, the sour water produced in treating processes can be directly used in the adjustment of the former system pH value of biochemical treatment, in whole treating processes, other sewage discharges are not had except moisture evaporation, therefore environmental protection pressure is die-offed, also without the need to again to danger useless processing mechanism payment process, cost for wastewater treatment is greatly reduced.In recycling process, certain salt is always had to be dissolved in mother liquor, cannot to separate out completely, the invention provides a kind of simple and effective treatment process for this reason, namely to filtrated stock and retain mother liquor mixed solution in add silicofluoric acid and make filtrated stock and retain mother liquor to change HCl and H into
2sO
4mixture, be directly used in the adjustment of system pH value before biochemical treatment, avoid complicated Recycling Mother Solution enrichment to divide salt process; The Sodium Silicofluoride of gained can also be sold as byproduct simultaneously, makes full use of waste water.
The present invention is according to the dissolubility property of nanofiltration membrane characteristic, sodium sulfate and sodium-chlor, the chemical property of silicofluoric acid and arranging especially, the sodium-chlor of 90% is by nanofiltration membrane, filtered liquid through nanofiltration membrane enters evaporative crystallization program, by controlling evaporation endpoint concentration, ensure a large amount of sodium-chlor crystallization.Significantly increase along with the rising of temperature when the solubleness of sodium sulfate is below about 40 DEG C, and reduce along with the rising of temperature time more than this temperature, though the solubleness of sodium-chlor increases with temperature and slightly increases, the impact by temperature is little.Therefore, during reclaim(ed) sulfuric acid sodium, adopt first by without the trapped fluid evaporation concentration of nanofiltration membrane, then crystallization sodium sulfate crystal at relatively high temperatures, by controlling evaporation endpoint concentration, ensure evaporation endpoint concentration drop on sodium sulfate crystallizing field, do not have sodium-chlor to separate out, thus obtain highly purified sodium sulfate.
The present invention adopts nanofiltration membrane directly sodium-chlor and sodium sulfate to be separated, and compared easier with adopting repeatedly evaporative crystallization in the past with the recovery method of cooling crystallization, the purity of two kinds of salt of crystallization gained is all improved.The filtered liquid simultaneously separated by nanofiltration membrane and trapped fluid can simultaneously by evaporative crystallization separately crystallization go out sodium-chlor and sodium sulfate, in step different from the past, first evaporative crystallization separates out a kind of salt, go to separate out another kind of salt to the evaporative crystallization that surplus solution carries out next step again, this strict sequencing causes inefficiency, the whole process of the present invention saves the time of 1/4th than existing recovery and treatment method, raises the efficiency.
Nanofiltration membrane is adopted to carry out filtration treatment to high-salt wastewater in steps A, the mould material of the membrane module of nano-filtration unit is polymeric amide material, membrane pore size is at below 2nm, feeding liquid side, high-salt wastewater pH2 ~ 11, wastewater temperature 4 ~ 45 DEG C, working pressure 0.5 ~ 1.5MPa, guarantee within the scope of nanofiltration membrane ability to bear, avoid the performance damaging film, more effectively can carry out solute classification.
Multiple-effect evaporator is adopted, any one when not having crystallization in optional falling-film evaporator, natural-circulation evaporator, pump feed evaporator, preferred falling-film evaporator in step B and C.Falling-film evaporator has very high heat interchanging area and good heat exchange property, and solution circulated amount is very little, is applicable to very much the large single vaporization step of steam output, effectively can accelerates velocity of evaporation, reduces evaporation cost.
Pump feed evaporator is selected when there being crystallization, pump feed evaporator is the vaporizer that a kind of heat transfer coefficient is large, resistive connection scar ability is strong, the forced-flow that the circulation of solution in equipment mainly relies on additionaling power to produce, speed of circulation generally can reach 1.5 ~ 5 meter per seconds; Heated when circulating liquid flows through heating chamber, then part evaporation when pressure reduces in separate chamber, by the boiling temperature under liquid cooling to corresponding pressure, due to the reason of recycle pump, the operation of pump feed evaporator and temperature are substantially irrelevant, the recirculation rate of material can fine adjustment, and vaporator rate setting within the specific limits; Feed liquid enters separator and is separated, can idetified separation effect, makes integral device have larger separation elasticity; The crystal that evaporation is separated out can by regulating circulation flow rate and adopting special separator designs to separate from loop slurry, be conducive to processing that viscosity is comparatively large, easily fouling, the material of easily crystallization or the higher solution of concentrating degree, therefore be highly suitable for evaporative crystallization steps to use, sodium-chlor effectively can be separated with sodium sulfate crystal.
The crystallizer that step B, step C use be selected from Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer and mutation thereof any one, be preferably provided with the vertical draft tube baffle crystallizer eluriating leg.Draft tube baffle crystallizer is a kind of typical magma inner circulation type crystallizer, has good fluid dynamic effect; Pressure head needed for its internal recycle is very low, water screw or propeller pump work under lower rotating speed, thus greatly reduce the secondary nucleation that the collision of impeller to crystal bring, and then ensure that the crystal produced in crystallizer has comparatively volume particle size, and size-grade distribution is good, seldom occur that inwall scabs phenomenon; The draft tube baffle crystallizer operational cycle is long, energy consumption is low, reliable, fault is few.Be provided with the vertical draft tube baffle crystallizer eluriating leg and can realize continuous seepage operation, realize the circulation and stress process to high-salt wastewater.Vertical elutriation leg can carry out counter flow washing when extraction crystal with stock liquid, ensures that the crystal of extraction contains impurity minimum, to reach technical grade quality standard.
Accompanying drawing explanation
Fig. 1 is the step for the treatment of process of the present invention and the schematic diagram of separated product;
Fig. 2 is the concrete technology schematic flow sheet of embodiment;
Wherein, 1, water feeder, 2, receive membrane module, 3, one effect heating chamber A, 4, one effect separate chamber A, 5, two effect heating chamber A, 6, two effect crystallizer A, 7, mother liquor pond, 8, whizzer A, 9, mother liquor tank, 10, whizzer B, 11, condensate water pot, 12, indirect condenser, 13, one effect heating chamber B, 14, one effect separate chamber B, 15, two effect heating chamber B, 16, two effect crystallizer B, 17, whizzer C, 18, steam input pipe road, 19, crystal output channel A, 20, raw steam condensate output channel, 21, high-salt wastewater input channel, 22, crystal output channel B, 23, crystal output channel C, 24, silicofluoric acid input channel, 25, recirculated water water supply pipeline, 26, recirculated water water return pipeline, 27, condensate output transistor road, 28, sour water output channel.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details:
The recovery and treatment method of the high-salt wastewater of sodium chloride-containing and sodium sulfate, high-salt wastewater containing sodium-chlor and sodium sulfate passes through nanofiltration membrane, filtered liquid through nanofiltration membrane obtains sodium-chlor and filtrated stock through evaporative crystallization, trapped fluid not through nanofiltration membrane obtains sodium sulfate and retain mother liquor through evaporative crystallization, filtrated stock adds silicofluoric acid wherein with retaining after mother liquor mixes, filter to obtain Sodium Silicofluoride after abundant stirring, the sour water after filtration is for the adjustment of system pH value before biochemical treatment.
A, nanofiltration membrane
High-salt wastewater is pumped into the feeding liquid side of nano-filtration unit, the operational condition of nano-filtration unit is: feeding liquid side, and wastewater pH is 2 ~ 11, wastewater temperature 4 ~ 45 DEG C, working pressure 0.5 ~ 1.5MPa, feeding liquid side crossflow velocity 1 ~ 2m/s.Be divided into through the filtered liquid of nanofiltration membrane with not through the trapped fluid of nanofiltration membrane through nanofiltration membrane by high-salt wastewater, 90% sodium-chlor through nanofiltration membrane, therefore mainly can contain sodium-chlor in filtered liquid, main containing sodium sulfate and a small amount of sodium-chlor in trapped fluid.
Filtered liquid is sent into step B process, trapped fluid sends into step C process;
B, filtered liquid evaporative crystallization
Filtered liquid is sent into evaporative crystallization section and carry out evaporation concentration, evaporation concentration temperature is 50 DEG C ~ 150 DEG C; Along with the continuous evaporation of water, the crystallization gradually of the sodium-chlor in filtered liquid, when in residual solution, solid-to-liquid ratio reaches 2% ~ 30%, sodium-chlor is separated out completely substantially; At 30 DEG C ~ 50 DEG C temperature, carry out solid-liquid separation, and with clear water, solid is washed, obtain highly purified sodium chloride crystal and filtrated stock.
The direct extraction of gained sodium chloride crystal, after drying process, its purity reaches technical grade, and can again use as industrial chlorinations sodium or directly sell as byproduct, remaining filtrated stock enters step D.
In this step, evaporation concentration temperature preferably 50 ~ 100 DEG C; The residual solution solid content of evaporation terminal is preferably 15% ~ 25%.
C, trapped fluid evaporative crystallization
Trapped fluid is sent into evaporative crystallization section and carry out evaporation concentration, evaporation concentration temperature is 50 ~ 150 DEG C; In this process, the moisture evaporation in trapped fluid, the concentration of wherein salt is raised gradually until separate out, and the crystal of now separating out is sodium sulfate; After the solid content in residual solution reaches 2% ~ 30%, the most of sodium sulfate crystallization all in trapped fluid, sodium-chlor still stays in the liquid phase.Under 50 ~ 100 DEG C of conditions, carry out solid-liquid separation, obtain highly purified sodium sulfate crystal and retain mother liquor;
First the sodium sulfate crystal of separating out in evaporation and crystal process is eluriated with high-salt wastewater in the elutriation leg of crystallizer, then washs gained solid with clear water in solid-liquid separation, finally obtains highly purified sodium sulfate crystal, directly extraction.After the sodium sulfate crystal drying process of extraction, its purity reaches technical grade quality, can again use as industrial sulphuric acid sodium or directly sell as byproduct.
Gained retains mother liquor and also enters step D.
In this step, evaporation concentration temperature preferably 70 ~ 100 DEG C; The residual solution solid content of evaporation terminal is preferably 15% ~ 25%; Solid-liquid separation temperature preferably 60 ~ 80 DEG C.
D, chemical precipitation
By filtrated stock with retain after mother liquor fully mixes, pump into chemical precipitation unit, in filtrated stock and the mixed solution retaining mother liquor, add silicofluoric acid, uniform stirring, fully after reaction, carries out filtration and makes solid-liquid separation, obtain Sodium Silicofluoride precipitation and sour water, sour water is HCl and H
2sO
4mixture, be directly used in the adjustment of system pH value before biochemical treatment.
Owing to inevitably containing some organism in coal chemical industrial waste water, if the too high precipitation that will have influence on salt of organic content.Therefore, need to monitor high-salt wastewater, filtered liquid, trapped fluid, filtrated stock, the organic content retained in mother liquor in actual production process; When organic concentration is higher than 1000mg/L, gac need be used, activated coke adsorbs organism, or by catalyzed oxidation, trim process is carried out to organism, be down to after 100 ~ below 300mg/L until organic concentration, send into next treatment step again, namely high-salt wastewater after treatment returns in high-salt wastewater pond, filtered liquid after treatment enters in step B, trapped fluid after treatment enters in step C, after treatment retain mother liquor and filtrated stock mixing after enter in step D.Organism is processed to the purity and color and luster that both can ensure salinity, the normal use of nanofiltration membrane can be ensured again, more avoid because organism constantly adds up to cause the elevation of boiling point serious and affect evaporative process.Be adsorbed with organic gac or activated coke can deliver to boiler and burn.Due to filtered liquid, trapped fluid, filtrated stock with to retain the amount of mother liquor few, directly can also return biochemical sewage operation and reduce COD, avoid unnecessary lengthy and jumbled treatment process, more effectively can unify check processing to organism.
Embodiment:
As shown in Figure 2, trapped fluid evaporative crystallization section adopts economic benefits and social benefits following current flow process in the technical process of the present embodiment; 1st effective evaporator adopts falling-film evaporator, comprises an effect separate chamber B14 and effect heating chamber B13; 2nd effect evaporator adopts forced circulation evaporation crystallizer, comprises two effect crystallizer B16 and two effect heating chamber B15.Filtered liquid evaporative crystallization section adopts economic benefits and social benefits following current flow process; 1st effective evaporator adopts falling-film evaporator, comprises an effect separate chamber A4 and effect heating chamber A 3; 2nd effect evaporator adopts forced circulation evaporation crystallizer, comprises two effect crystallizer A6 and two effect heating chamber A 5.
Flow direction of material:
A, nanofiltration membrane
First high-salt wastewater from high-salt wastewater input channel 21 enters water feeder 1, then be admitted under the effect of feeding pump and receive membrane module 2 and carry out nanofiltration membrane, the operating environment of nanofiltration membrane is: pH=2 ~ 11 of high-salt wastewater, concentration is about 1wt%, wastewater temperature is 4 ~ 45 DEG C, and working pressure is 0.5 ~ 1.5MPa.Through nanofiltration membrane, high-salt wastewater is divided into through the filtered liquid (sodium-chlor) of nanofiltration membrane with not through the trapped fluid (a small amount of sodium-chlor and sodium sulfate mixture) of nanofiltration membrane, filtered liquid is sent into step B process, trapped fluid sends into step C process.
B, filtered liquid evaporative crystallization
Filtered liquid evaporative crystallization section adopts economic benefits and social benefits following current flow process; 1st effective evaporator adopts falling-film evaporator, and comprise an effect separate chamber A4 and effect heating chamber A 3, evaporation concentration temperature is set in 80 DEG C; 2nd effect evaporator adopts forced circulation evaporation crystallizer, and comprise two effect crystallizer A6 and two effect heating chamber A 5, evaporation concentration temperature is set in 80 DEG C, when solid-to-liquid ratio reaches 20% in residual solution, is delivered to whizzer A8 carries out concentrating and separating through two effect discharging pumps.Be separated to obtain sodium chloride crystal and filtrated stock, NaCl crystal through the direct extraction of crystal output channel B22, through washing drying treatment after namely can be used as finished product sell, it is stand-by that filtrated stock enters mother liquor pond 7.
C, trapped fluid evaporative crystallization
Trapped fluid evaporative crystallization section adopts economic benefits and social benefits following current flow process; 1st effective evaporator adopts falling-film evaporator, and comprise an effect separate chamber B14 and effect heating chamber B13, evaporation concentration temperature is 80 DEG C; 2nd effect evaporator adopts forced circulation evaporation crystallizer, and comprise two effect crystallizer B16 and two effect heating chamber B15, evaporation concentration temperature is 80 DEG C.When solid-to-liquid ratio reaches 20% in residual solution, be delivered to whizzer C17 through two effect discharging pumps and be separated.Be separated to obtain sodium sulfate crystal and retain mother liquor, sodium sulfate crystal through the direct extraction of crystal output channel A19, after washing drying treatment, namely can be used as finished product sell, retaining mother liquor, to enter mother liquor pond 7 stand-by.
D, chemical precipitation
In mother liquor pond 7, silicofluoric acid is added by silicofluoric acid input channel 24, whizzer B10 is pumped into after abundant stirring reaction is complete, filter gained Sodium Silicofluoride by the direct extraction of crystal output channel C23, residual acid water delivery pipe road 28 returns biochemical front system fading margin pH value;
Steam and condensation flow to:
The shell side that steam enters an effect heating chamber A 3 and an effect heating chamber B13 respectively by steam input pipe road 18 carries out heat exchange condensation, discharges after the mixing of the two water of condensation through raw steam condensate output channel 20; The shell side that the secondary vapour produced by an effect separate chamber A4 and effect separate chamber B14 enters two effect heating chamber A 5 and two effect heating chamber B15 respectively carries out heat exchange condensation, and water of condensation enters condensate water pot 11 and keeps in; Two effect crystallizer A6 and two are imitated the secondary vapour that crystallizer B16 produces and enter condensate water pot 11 after indirect condenser 12 condensations.Water of condensation in condensate water pot 11 is driven by condensate pump, is discharged by condensate output transistor road 27 again, recycles further.Two effect crystallizer A6 and two imitate secondary vapour that crystallizer B16 produces after indirect condenser 12 condensation, and noncondensable gas is extracted out by vacuum pump, enters air.
Circulating water flow to:
After the recirculated water carrying out self-circulating water water supply pipeline 25 enters indirect condenser 12 heat exchange, directly discharge through recirculated water water return pipeline 26.
The present invention adopts nanofiltration membrane directly sodium-chlor and sodium sulfate to be separated, compared easier with adopting repeatedly evaporative crystallization in the past with the recovery method of cooling crystallization, the purity of two kinds of salt of crystallization gained is all improved, the massfraction of sodium-chlor reaches 95.9%, and the massfraction of sodium sulfate reaches 96.2%.The filtered liquid simultaneously separated by nanofiltration membrane and trapped fluid can simultaneously by evaporative crystallization separately crystallization go out sodium-chlor and sodium sulfate, in step different from the past, first evaporative crystallization separates out a kind of salt, go to separate out another kind of salt to the evaporative crystallization that surplus solution carries out next step again, this strict sequencing causes inefficiency, the whole process of the present invention saves the time of 1/4th than existing recovery and treatment method, raises the efficiency.
The inventive method is a kind for the treatment of process of iterative cycles, the sour water produced in treating processes can be directly used in the adjustment of the former system pH value of biochemical treatment, in whole treating processes, other sewage discharges are not had except moisture evaporation, therefore environmental protection pressure is die-offed, also without the need to again to danger useless processing mechanism payment process, cost for wastewater treatment is greatly reduced.In recycling process, certain salt is always had to be dissolved in mother liquor, cannot to separate out completely, the invention provides a kind of simple and effective treatment process for this reason, namely to filtrated stock and retain mother liquor mixed solution in add silicofluoric acid and make filtrated stock and retain mother liquor to change HCl and H into
2sO
4mixture, be directly used in the adjustment of system pH value before biochemical treatment, avoid complicated Recycling Mother Solution enrichment to divide salt process; The Sodium Silicofluoride of gained can also be sold as byproduct simultaneously, makes full use of waste water.
The sodium sulfate crystal of this technique institute extraction and sodium chloride crystal, after super-dry, carry out Performance Detection, detected result is respectively in table 1, table 2.
Table 1 sodium sulfate product performance detect
| Project | Embodiment 1 sodium sulfate product | Technical grade sodium sulfate performance index |
| Sodium sulfate quality mark | 96.2％ | III class acceptable end product: 95% |
Table 2 sodium-chlor product performance detect
| Project | Embodiment 1 sodium-chlor product | Technical grade sodium-chlor performance index |
| Sodium-chlor massfraction | 95.9％ | One-level Exposure to Sunlight Industrial Salt: 94.5% |
Can be found out by above data, the sodium sulfate product obtained by the inventive method, sodium-chlor product reach the performance requriements of technical grade sodium sulfate, technical grade sodium-chlor respectively, can sell as technical grade product.
Claims (10)
1. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing and sodium sulfate, it is characterized in that: the high-salt wastewater containing sodium-chlor and sodium sulfate passes through nanofiltration membrane, filtered liquid through nanofiltration membrane obtains sodium-chlor and filtrated stock through evaporative crystallization, trapped fluid not through nanofiltration membrane obtains sodium sulfate and retain mother liquor through evaporative crystallization, filtrated stock adds silicofluoric acid wherein with retaining after mother liquor mixes, filter to obtain Sodium Silicofluoride after abundant stirring, the sour water after filtration is for the adjustment of system pH value before biochemical treatment.
2. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 1 and sodium sulfate, is characterized in that concrete steps are:
A, nanofiltration membrane
High-salt wastewater is pumped into the feeding liquid side of nano-filtration unit, through nanofiltration membrane, high-salt wastewater is divided into through the filtered liquid of nanofiltration membrane with not through the trapped fluid of nanofiltration membrane;
Described filtered liquid enters step B process, and described trapped fluid enters step C process;
B, filtered liquid evaporative crystallization
Sent into by filtered liquid in evaporative crystallizer and carry out evaporation concentration and obtain sodium-chlor and filtrated stock, evaporation concentration temperature is 50 ~ 150 DEG C;
The direct extraction of described sodium chloride crystal, filtrated stock enters step D process;
C, trapped fluid evaporative crystallization
Trapped fluid is sent into evaporative crystallizer and carry out evaporation concentration, evaporation concentration temperature is 50 ~ 150 DEG C, after the solid content of solution reaches 2% ~ 30%, stops evaporation; Under 50 ~ 100 DEG C of conditions, carry out solid-liquid separation, obtain sodium sulfate crystal and retain mother liquor;
The direct extraction of described sodium sulfate crystal, retains mother liquor and enters step D process;
D, chemical precipitation
By filtrated stock with retain after mother liquor fully mixes, pump into chemical precipitation unit, in filtrated stock and the mixed solution retaining mother liquor, add silicofluoric acid, uniform stirring, fully after reaction, carry out filtration and make solid-liquid separation, obtain Sodium Silicofluoride precipitation and sour water;
Described Sodium Silicofluoride is directly extraction after filtration, and the sour water after filtration is for the adjustment of system pH value before biochemical treatment.
3. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 2 and sodium sulfate, it is characterized in that: in described steps A, the operating environment of nanofiltration membrane is: pH=2 ~ 11 of high-salt wastewater, concentration is about 1wt%, wastewater temperature is 4 ~ 45 DEG C, and working pressure is 0.5 ~ 1.5MPa;
The mould material of the membrane module of described nano-filtration unit is polymeric amide material, and membrane pore size is less than 2nm.
4. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 1 and sodium sulfate, it is characterized in that: detect high-salt wastewater respectively, filtered liquid, trapped fluid, filtrated stock, retain the organism in mother liquor, work as high-salt wastewater, filtered liquid, trapped fluid, filtrated stock, when retaining organic concentration in mother liquor in any one liquid more than 1000mg/L, charcoal absorption is used to exceed standard the organism in solution or processed the organism exceeded standard in solution by catalyzed oxidation, treat that organic concentration is down to 100 ~ below 300mg/L and is entered next treatment step again.
5. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 1 and sodium sulfate, it is characterized in that: be detected filtrate, trapped fluid, filtrated stock, the organism retained in mother liquor respectively, when filtered liquid, trapped fluid, filtrated stock, the organic concentration retained in mother liquor in any one liquid directly send biochemical wastewater treatment operation back to more than during 1000mg/L.
6. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 2 and sodium sulfate, it is characterized in that: the Sodium Silicofluoride of the sodium sulfate crystal of the sodium chloride crystal of step B extraction, step C extraction, step D filtration gained is carried out washing and drying treatment respectively, makes sodium sulfate crystal, sodium chloride crystal and Sodium Silicofluoride reach the quality standard of technical grade sodium sulfate, technical grade sodium-chlor, technical grade Sodium Silicofluoride respectively.
7. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 2 and sodium sulfate, it is characterized in that: described evaporative crystallizer comprises vaporizer and crystallizer, vaporizer is any one in natural-circulation evaporator, falling-film evaporator, pump feed evaporator.
8. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 7 and sodium sulfate, is characterized in that: described vaporizer is single-effect evaporator, multiple-effect evaporator, MVR vaporizer or TVR vaporizer.
9. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 7 and sodium sulfate, is characterized in that: crystallizer is any one in the mutation of Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer and above pattern.
10. the recovery and treatment method of the high-salt wastewater of sodium chloride-containing according to claim 9 and sodium sulfate, is characterized in that: described crystallizer is provided with the vertical crystallizer eluriating leg.
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