CN105036222A - High-salinity wastewater recovery treatment method - Google Patents
High-salinity wastewater recovery treatment method Download PDFInfo
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Abstract
The invention discloses a high-salinity wastewater recovery treatment method. The method is characterized by recovering sodium sulfate, sodium chloride and sodium nitrate through four treatment steps, namely primary evaporative crystallization, cooling crystallization, secondary evaporative crystallization and freezing crystallization. The method has the beneficial effects that sodium chloride, sodium sulfate and sodium nitrate in high-salinity wastewater can be respectively recovered; obtained sodium chloride, sodium sulfate and sodium nitrate achieve the industrial level and can be directly recovered and reused or be sold as byproducts, thus not only achieving the aim of treating high-salinity wastewater and meeting the current situation requirement of environmental protection but also turning waste into wealth, achieving resource utilization of salt and increasing the profits of factories.
Description
Technical field
The present invention relates to the treatment process of waste water, especially a kind of recovery and treatment method of coal chemical industry high-salt wastewater.
Background technology
China is oil-poor, the energy structure of weak breath, many coals determines the main energy sources that coal remains China's present stage, and coal chemical industry can extract various product from coal, makes full use of the value of coal.Along with the development of coal chemical industry, also bring a new difficult problem, the generation of coal chemical industry high slat-containing wastewater constrains the continuation development of Coal Chemical Industry, also result in very large environmental pollution and the wasting of resources.
High-salt wastewater refers to that total dissolved solidss and organic mass content are more than or equal to the waste water of 1.0%, comprises high salt sanitary wastewater and high salt industrial waste water.The main source of high-salt wastewater is the sewage directly utilizing the industrial production of seawater and sanitary sewage and food processing plant, pharmaceutical factory, chemical plant, petroleum collection processing industry, Sweet natural gas collection processing industry etc. to produce.The waste water that these sewage obtain after biochemical treatment is high-salt wastewater, except containing organic contamination beyond the region of objective existence in high-salt wastewater, also containing a large amount of inorganic salt, as Cl
-, SO
4 2-, Na
+, Ca
2+, NO
4 -plasma.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.
About the treatment technology of high-salt wastewater, have studied decades both at home and abroad, the method usually adopted at present mainly comprises biological treatment, ion exchange method, chemical precipitation method and evaporative desalination method etc.Ion exchange method can reach the object of desalination to a certain extent, but often loses effect because of the suspended solid blocking resin in waste water, and in addition, this method is expensive and the refuse exchanged is difficult to process.Chemical precipitation method is a kind of traditional water treatment method, technology is comparatively ripe, less investment, and process is simple, only need to add medicament, but the more difficult control of the addition of medicament, medicament is too much, introduces other impurity to waste water, medicament is too low, cannot reach the object of process waste water, in addition, in processed waste water, how throw out processes also is one of its factor developed of restriction.
In numerous high-salt wastewater treatment technologies, evaporative desalination method possess skills maturation, the advantages such as waste water scope is wide, processing speed is fast, energy-conservation can be processed, thus there is larger development prospect at home.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 evaporative desalination method to separate out is all the mixed salt simultaneously comprising multiple salt, purity is low, cannot industrially reuse, usually mixed salt directly discarded or give the useless processing mechanism of danger to carry out professional treatment with the price of 300 ~ 5000 yuan per ton, not only increase environmental protection pressure like this, also considerably increase the cost for wastewater treatment of factory.
The sewage produced in Coal Chemical Industry production process, through biochemical treatment with filter out impurities, sodium sulfate, sodium-chlor, SODIUMNITRATE three kinds of salt are mainly comprised in remaining high-salt wastewater, the mixed salt of these three kinds of salt is very difficult to process, and these three kinds of salt usage quantity is industrially very large, discards in vain unfortunately.Therefore, the sodium sulfate, sodium-chlor and the SODIUMNITRATE that reclaim in high-salt wastewater are significant.
Summary of the invention
The technical issues that need to address of the present invention are to provide a kind of recovery and treatment method of the high-salt wastewater for coal chemical industry generation, effectively can be recycled the sodium sulfate in high-salt wastewater, sodium-chlor and SODIUMNITRATE by the method, greatly reduce environmental protection pressure and cost for wastewater treatment.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A recovery and treatment method for high-salt wastewater, by single vaporization crystallization, cooling crystallization, double evaporation-cooling crystallization, freezing and crystallizing four treatment step reclaim(ed) sulfuric acid sodium, sodium-chlor and SODIUMNITRATE.
The further improvement of technical solution of the present invention is: the concrete steps of described treatment process are,
A, single vaporization crystallization
High-salt wastewater is sent into single vaporization crystallizer to carry out single vaporization and concentrate, thickening temperature is 50 ~ 150 DEG C, be concentrated to crystallization and the solid content of remaining liq is 2 ~ 30% time, at 50 ~ 100 DEG C, carry out solid-liquid separation, obtain sodium sulfate crystal and a mother liquor;
The direct extraction of described sodium sulfate crystal, one time mother liquor enters step B process; At the elutriation leg high-salt wastewater of crystallizer, solid is eluriated, again gained solid is washed at solid-liquid separation process clear water;
B, cooling crystallization
A mother liquor is carried out low temperature crystallization and carries out solid-liquid separation, and recrystallization temperature is-15 ~ 0 DEG C, obtains the mixed salt, the cooling mother liquor that include sal glauberi and two water sodium-chlor;
Described mixed salt is again sent dissolving in high-salt wastewater back to, is carried out circulation and stress process, and cooling mother liquor enters step C process;
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out double evaporation-cooling concentrate, thickening temperature is 50 ~ 150 DEG C, along with the evaporation of moisture, sodium-chlor crystallization in cooling mother liquor and the solid content of remaining liq are when reaching 2 ~ 30%, at 30 ~ 50 DEG C, carry out solid-liquid separation, obtain sodium chloride crystal and secondary mother liquid;
The direct extraction of described sodium chloride crystal, secondary mother liquid enters step D process; At the elutriation leg cooling mother liquor of crystallizer, solid is eluriated, again gained solid is washed at solid-liquid separation process clear water;
D, freezing and crystallizing
Secondary mother liquid is carried out cryogenic freezing crystallization and carries out solid-liquid separation, Tc is-15 ~ 0 DEG C, obtains SODIUMNITRATE crystal and freezing mother liquor;
The direct extraction of described SODIUMNITRATE crystal, freezing mother liquor returns biochemistry pool, and the nitrogenous source as biochemistry pool supplements.
The further improvement of technical solution of the present invention is: when the organic concentration in described high-salt wastewater, mother liquor, cooling mother liquor, secondary mother liquid and freezing mother liquor is higher than 1000mg/L, directly send biochemical wastewater treatment operation back to, or use gac or catalyzed oxidation to process organism, treat that organic concentration is reduced to below 1000mg/L and enters next treatment step again.
The further improvement of technical solution of the present invention is: the SODIUMNITRATE crystal of the sodium sulfate crystal of described steps A extraction, the sodium chloride crystal of step C extraction, step D extraction, after washing accordingly and drying treatment, reaches the quality standard of technical grade sodium sulfate, technical grade sodium-chlor, technical grade SODIUMNITRATE respectively.
The further improvement of technical solution of the present invention is: described single vaporization crystallizer comprises single vaporization device and primary crystallization device, described double evaporation-cooling crystallizer comprises second evaporator and secondary crystal device, and described single vaporization device is the one in the array configuration of a kind of or above-mentioned vaporizer in natural-circulation evaporator, falling-film evaporator, pump feed evaporator, MVR vaporizer, TVR vaporizer.
The further improvement of technical solution of the present invention is: when in described single vaporization process, double evaporation-cooling process, nodeless mesh is separated out, single vaporization device, second evaporator are falling-film evaporator or natural-circulation evaporator, when having crystallization in single vaporization process, double evaporation-cooling process, single vaporization device, second evaporator are pump feed evaporator.
The further improvement of technical solution of the present invention is: described single vaporization device and second evaporator are respectively single-effect evaporator, multiple-effect evaporator, MVR vaporizer or TVR vaporizer.
The further improvement of technical solution of the present invention is: the freezing and crystallizing device used in the cooling crystallization device used in described primary crystallization device, step B, secondary crystal device, step D is any one in Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer respectively.
The further improvement of technical solution of the present invention is: described step crystallization device 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 a kind of recovery and treatment method of high-salt wastewater, reclaim for the high-salt wastewater produced processes such as Coal Chemical Industries, processing condition simple and stable.Pass through the inventive method, sodium-chlor in high-salt wastewater, sodium sulfate and SODIUMNITRATE can be reclaimed respectively, the sodium-chlor obtained, sodium sulfate and SODIUMNITRATE reach technical grade level, can direct recovery or sell as byproduct, not only reach the object of process high-salt wastewater, meet current Environmental Protection Situation needs, and turn waste into wealth, achieve the recycling of salt, improve the income of factory.
The inventive method is circulation process method, circulation and stress process in high-salt wastewater got back to by the mixed salt produced in process, freezing mother liquor gets back to double evaporation-cooling Crystallization Procedure, outside whole process is evaporated apart from moisture, there is no other sewage discharges, 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, for being dissolved in the salt cannot separated out completely in mother liquor, finally being separated out by continuous enrichment, achieving salt in high-salt wastewater and reclaim to greatest extent.
The present invention is dissolubility property according to sodium sulfate, sodium-chlor and SODIUMNITRATE and arranges especially.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 high-salt wastewater evaporation concentration, then separate out sodium sulfate crystal at relatively high temperatures, by controlling evaporation endpoint concentration, ensure that evaporation endpoint concentration drops on the crystallizing field of sodium sulfate, do not have sodium-chlor to separate out, thus obtain highly purified sodium sulfate.A mother liquor after centrifugation sodium sulfate is again by the mixed salt of separating out sodium sulfate and sodium-chlor that cools, the sodium sulfate that further removing is remaining, sodium-chlor in remaining cooling mother liquor after solid-liquid separation, SODIUMNITRATE content are very high, the sodium sulfate only containing extremely trace.
The present invention is according to the characteristic of sodium-chlor and SODIUMNITRATE solvability binary phase diagram, and under high temperature, SODIUMNITRATE cementing degree is very high, and sodium-chlor temperature influence is not obvious, therefore, the double evaporation-cooling crystallization under high temperature of cooling mother liquor, subsequent filtration is obtained highly purified sodium-chlor.By controlling evaporation endpoint concentration, ensureing that evaporation endpoint concentration drops on the crystallizing field of sodium-chlor, not having SODIUMNITRATE and sodium sulfate to separate out.In secondary mother liquid after Isolating chlorinated sodium, Main Salts is SODIUMNITRATE, and now make mother liquor freezing and crystallizing under low temperature obtain high pure nitric acid sodium, freezing mother liquor returns double evaporation-cooling Crystallization Procedure circular treatment.Moving in circles through said process, can make the sodium sulfate of the overwhelming majority in high-salt wastewater, sodium-chlor and SODIUMNITRATE be recycled.
High-salt wastewater of the present invention is after single vaporization crystallization, and heat filtering under comparatively high temps, obtains highly purified sodium sulfate; A mother liquor cooling crystallization obtains the mixed salt of sodium sulfate and sodium-chlor, removes sodium sulfate further, and mixed salt returns feed reservoir and regulates Cl
-and SO
4 2-ion ratio; The double evaporation-cooling crystallization under high temperature of gained cooling mother liquor, heat filtering obtains high-purity sodium-chlor subsequently; After secondary mother liquid evaporative crystallization, under low temperature, freezing and crystallizing filters and obtains high-purity SODIUMNITRATE.This technology adopts eluriates leg formula evaporative crystallizer, and available mother liquor or stock liquid carry out back flushing to it, and the crystal grain ensureing extraction is evenly and containing less impurity.
In the present invention, organism is processed, both can ensure purity and the color and luster of salinity, make salinity reach technical grade standard, can avoid again because organism constantly adds up to cause the elevation of boiling point serious and affect evaporative process.
When adopting multiple-effect evaporator in steps A, any one when not having crystallization in optional falling-film evaporator, natural-circulation evaporator, pump feed evaporator, preferred falling-film evaporator.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.
Double evaporation-cooling crystallizer in step C select in pump feed evaporator, scrapper thin film evaporator any one, preferred pump feed evaporator.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, and 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 double evaporation-cooling step to use, sodium chloride crystal effectively can be separated.
The freezing and crystallizing device used in the cooling crystallization device used in primary crystallization device in the present invention, step B, secondary crystal device, step D be selected from Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer and mutation pattern thereof any one, be preferably provided with the vertical draft tube baffle crystallizer and mutation thereof of eluriating leg.Draft tube baffle crystallizer and mutation pattern thereof are a kind of typical magma inner circulation type crystallizers, have 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.
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 1;
Wherein, 1, preheater, 2, one effect heating chamber, 3, one effect separate chamber, 4, two effect heating chambers, 5, two effect fractional crystallization devices, 6, a whizzer, 7, a mother liquor tank, 8, jacketed type cooling stirring tank, 9, cooling crystallization whizzer, 10, cooling main flow container, 11, triple effect heating chamber, 12, triple effect fractional crystallization device, 13, indirect condenser, 14, condensate water pot, 15, secondary centrifuging machine, 16, secondary mother liquid tank, 17, Outer Cooler, 18, Oslo crystallizer, 19, thickener, 20, freezing and crystallizing whizzer, 21 freezing mother liquor tanks, 22, high-salt wastewater feed pipe, 23, condensate output transistor road I, 24, steam input pipe road, 25, chilled brine input channel, 26, sodium sulfate discharge pipe, 27, condensate output transistor road, 28, sodium-chlor discharge pipe, 29, recirculated water water supply pipeline, 30, recirculated water water return pipeline, 31, chilled brine output channel, 32, SODIUMNITRATE discharge pipe.
Black arrow in Fig. 2 represents the trend of high-salt wastewater, and double-headed arrow represents the trend of water coolant, refrigerated water, steam, water of condensation.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further details:
A recovery and treatment method for high-salt wastewater, as shown in Figure 1, by single vaporization crystallization, cooling crystallization, double evaporation-cooling crystallization, freezing and crystallizing four treatment step reclaim(ed) sulfuric acid sodium, sodium-chlor and SODIUMNITRATE.
The concrete steps of this recovery and treatment method are:
A, single vaporization crystallization
High-salt wastewater is sent into after preheating single vaporization crystallizer and carry out evaporation concentration, thickening temperature is about 50 ~ 150 DEG C; In this process, the water evaporation in high-salt wastewater, the concentration of wherein salt is raised gradually until separate out, and the crystal of now separating out is sal glauberi; When the solid content being evaporated to remaining liq is 2 ~ 30%, the most of sodium sulfate crystallization gradually in high-salt wastewater, and sodium-chlor and SODIUMNITRATE are still stayed in the liquid phase.Carry out solid-liquid separation under 50 ~ 100 DEG C of conditions after, obtain highly purified sodium sulfate crystal and a mother liquor;
The sodium sulfate crystal of separating out in single vaporization crystallisation process, first eluriates solid at the elutriation leg high-salt wastewater of crystallizer, then washs gained solid at solid-liquid separation process clear water again.The direct extraction of the highly purified sodium sulfate crystal of gained, after drying process, its purity reaches technical grade, can again use as industrial sulphuric acid sodium or directly sell as byproduct.
In gained mother liquor, the content of sodium sulfate is lower, sends into step B and is further processed, the concentration ratio of sodium-chlor and sodium sulfate in adjustment mother liquor.
In this step, single vaporization thickening temperature preferably 50 ~ 100 DEG C, most preferably 75 DEG C.The solid content being evaporated to remaining liq is preferably 10 ~ 30%, and most preferably 20%.Solid-liquid separation temperature preferably 60 ~ 80 DEG C, most preferably 70 DEG C.
B, cooling crystallization
Mother liquor is sent into cooling crystallizer to lower the temperature further crystallization, recrystallization temperature is-15 DEG C ~ 0 DEG C; Along with temperature reduces, remaining most of sodium sulfate and partial oxidation sodium can together with crystallization; Keep-15 DEG C ~ 0 DEG C to carry out solid-liquid separation process, obtain mixed salt and cooling mother liquor.
Described mixed salt is again sent back in high-salt wastewater to dissolve and continue circulation and is recycled.
In described cooling mother liquor sodium-chlor and sodium nitrate concentration very high, the content of sodium sulfate is reduced to 0.44% ~ 1.2% further, ensures to enter the crystallizing field of sodium-chlor by evaporation, is admitted to step C and is further processed.
In this step, recrystallization temperature preferably-10 DEG C ~-2 DEG C, most preferably-5 DEG C.Solid-liquid separation temperature preferably-10 DEG C ~-2 DEG C, most preferably-5 DEG C.
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out double evaporation-cooling concentrate, thickening temperature is 50 DEG C ~ 150 DEG C, ensure the crystallizing field being entered sodium-chlor by evaporation, along with the continuous evaporation of water, sodium-chlor in mother liquor to be cooled crystallization gradually, when the solid content being evaporated to remaining liq is 2 ~ 30%, sodium-chlor is separated out completely substantially; Through solid-liquid separation process at 30 DEG C ~ 50 DEG C temperature, obtain sodium chloride crystal and secondary mother liquid;
The sodium chloride crystal of separating out in double evaporation-cooling crystallisation process, first eluriates solid at the elutriation leg cooling mother liquor of crystallizer, then washs gained solid at solid-liquid separation process clear water again.The direct extraction of gained sodium chloride crystal, after drying process, its purity reaches technical grade, can again use as industrial chlorinations sodium or directly sell as byproduct.
In described secondary mother liquid, sodium nitrate concentration is very high, and sodium sulfate and sodium chloride content are extremely low, is admitted to step D and is further processed.
In this step, double evaporation-cooling thickening temperature preferably 80 ~ 120 DEG C, most preferably 100 DEG C.The solid content being evaporated to remaining liq is preferably 10 ~ 30%, and most preferably 20%.Solid-liquid separation temperature preferably 30 ~ 40 DEG C, most preferably 30 DEG C.
D, freezing and crystallizing
Secondary mother liquid is sent into freezing and crystallizing device and carry out freezing and crystallizing, Tc is-15 DEG C ~ 0 DEG C; Along with temperature reduces, SODIUMNITRATE crystallization; Through solid-liquid separation process, obtain SODIUMNITRATE crystal and freezing mother liquor;
The direct extraction of gained SODIUMNITRATE crystal, after drying process, its purity reaches technical grade, can again use as industrial sodium nitrate or directly sell as byproduct.In described freezing mother liquor or the common saturated solution of three, in order to thoroughly reclaim product salt wherein, therefore freezing mother liquor is again sent back in double evaporation-cooling operation, is continued circulation and recycle.
In this step, Tc preferably-15 DEG C ~-5 DEG C, most preferably-10 DEG C.Solid-liquid separation temperature preferably-15 DEG C ~-5 DEG C, most preferably-10 DEG C.
In actual production process, when the low salinity in high-salt wastewater, salts contg are below 10%, if directly send into single vaporization Crystallization Procedure, the quantity of steam then evaporating consumption is large, steam expense is higher, in order to save evaporation energy consumption, MVR vaporizer first can be used to carry out pre-concentration to high-salt wastewater, make salts contg reach about 20%, send into single vaporization crystallizer again, effectively can reduce the energy consumption of circulating treatment procedure.
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, mother liquor, the organic content cooled in mother liquor, secondary mother liquid and freezing mother liquor in actual production process; When organic content is higher than 1000mg/L, then need to use gac, activated coke or catalysed oxidation processes to process organism, when organic concentration is down to below 1000mg/L, when can guarantee to obtain technical grade solid salt, enter next treatment step again, the gac of adsorb organic compound or activated coke can be delivered to boiler and burn.Mother liquor, cooling mother liquor, secondary mother liquid and freezing mother liquor, because amount is fewer, it is also conceivable to directly to return biochemical system process COD.
Embodiment 1
The present embodiment is the recovery processing technique of the high-salt wastewater containing sodium sulfate, sodium-chlor, SODIUMNITRATE, and technical process as shown in Figure 2.
In the present embodiment, single vaporization crystallization adopts economic benefits and social benefits following current flow process, and 1st effective evaporator adopts falling-film evaporator, comprises effect separate chamber 3 and an effect heating chamber 2.2nd effect evaporator adopts forced circulation evaporation crystallizer, comprises two effect fractional crystallization device 5 and two effect heating chambers 4.
Cooling crystallization adopts jacketed type cooling stirring tank 8, and refrigerant adopts chilled brine.
Double evaporation-cooling crystallization adopts single-action pump feed evaporator, comprises triple effect fractional crystallization device 12 and triple effect heating chamber 11.
Freezing and crystallizing operation adopts external-cooling type Oslo crystallizer, comprises Outer Cooler 17 and Oslo crystallizer 18.
Flow direction of material:
A, single vaporization crystallization
First high-salt wastewater in head tank enters preheater 1 by high-salt wastewater feed pipe 22, is sent to single vaporization Crystallization Procedure after preheating.First high-salt wastewater enters in the 1st effective evaporator of falling-film evaporator formation, carry out evaporation concentration, part feed liquid realizes effect internal recycle through an effect recycle pump, and another part feed liquid crosses the two effect evaporative crystallizers expecting that forced circulation evaporation crystallizer is formed, and continues evaporation concentration.When solid content to remaining liq to be evaporated is 20%, through the centrifugation of a whizzer 6, obtain sodium sulfate crystal and a mother liquor.Sodium sulfate crystal by sodium sulfate discharge pipe 26 directly extraction, after washing drying treatment, namely can be used as finished product sell, a mother liquor enters a mother liquor tank 7 and keeps in.
B, cooling crystallization
A mother liquor in a mother liquor tank 7 enters cooling crystallization operation, mother liquor through pump delivery to jacketed type cooling stirring tank 8, temperature is kept to be-15 DEG C ~ 0 DEG C, the mixed salt including sal glauberi and two water sodium-chlor along with temperature reduction together with crystallization, with after obtain mixed salt and cooling mother liquor through cooling crystallization whizzer 9 centrifugation.Mixed salt is sent back to head tank and dissolves, and in order to regulate sodium sulfate and sodium-chlor ratio in high-salt wastewater, and continues recycle; Cooling mother liquor enters cooling main flow container 10 and keeps in.
C, double evaporation-cooling crystallization
Cooling mother liquor in cooling main flow container 10 enters double evaporation-cooling Crystallization Procedure, further evaporative crystallization is carried out in the double evaporation-cooling crystallizer that pump delivery to single-action pump feed evaporator is formed, the solid content being evaporated to remaining liq is 20%, being delivered to secondary centrifuging machine 15 through triple effect discharging pump carries out centrifugal, is separated to obtain sodium chloride crystal and secondary mother liquid.Sodium chloride crystal through sodium-chlor discharge pipe 28 directly extraction, after washing drying treatment, namely can be used as finished product sell; Secondary mother liquid enters secondary mother liquid tank 16 and keeps in.
D, freezing and crystallizing
Secondary mother liquid in secondary mother liquid tank 16 enters freezing and crystallizing operation, freezing and crystallizing is carried out to being with the Oslo crystallizer 18 of Outer Cooler 17 through pump delivery, temperature is kept to be-15 DEG C ~ 0 DEG C, SODIUMNITRATE crystal is separated out gradually with the reduction of temperature, with after through thickener 19, the centrifugation of cold dynamic crystallizer centrifuge 20 obtains SODIUMNITRATE crystal and cold dynamic mother liquor.SODIUMNITRATE crystal through SODIUMNITRATE discharge pipe 32 directly extraction, after washing drying treatment, namely can be used as finished product sell; Cold dynamic mother liquor enters cold dynamic mother liquor tank 21.Recycle is continued, thoroughly to reclaim salt wherein by the cooling main flow container 10 of mother liquor pumped back double evaporation-cooling Crystallization Procedure.
Steam flow:
The shell side that steam enters an effect heating chamber 2 by steam input pipe road 24 carries out heat exchange condensation, and water of condensation enters the shell side preheating high-salt wastewater stock liquid of preheater 1 as thermal source, with after be delivered to other operation through condensate output transistor road I 23; The shell side that the secondary steam produced by an effect separate chamber 3 enters two effect heating chambers 4 carries out heat exchange condensation, and water of condensation enters triple effect heating chamber 11 and makes full use of as thermal source; The secondary steam that two effect fractional crystallization devices 5 produce is used for the thermal source of double evaporation-cooling Crystallization Procedure (i.e. triple-effect evaporator), sends into condensate water pot 14 with water of condensation after triple effect heating chamber 11 heat exchange through pipeline.
Condensation flow to:
Water of condensation in condensate water pot 14 again by pump drive, by condensate output transistor road II 27 export, recycle further.The secondary vapour that triple effect fractional crystallization device 12 produces is after indirect condenser 13 condensation, and noncondensable gas is extracted out by vacuum pump, enters air.
Chilled brine flows to:
Chilled brine from chilled brine input channel 25 enters cooling stirring tank 8 respectively and the shell side of Outer Cooler 17 carries out cooling down, then directly discharges through chilled brine output channel 31.
Circulating water flow to:
After the water coolant carrying out self-circulating water water supply pipeline 29 enters indirect condenser 13 heat exchange, directly discharge through recirculated water water return pipeline 30.
The sodium sulfate crystal of this technique institute extraction, sodium chloride crystal and SODIUMNITRATE crystal, after washing drying, carry out Performance Detection, detected result is respectively in table 1, table 2, table 3.
Table 1 sodium sulfate product performance detect
| Project | Embodiment 1 sodium sulfate product | Technical grade sodium sulfate performance index |
| Sodium sulfate quality mark | 95.8％ | 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 | 95.2％ | Secondary Exposure to Sunlight Industrial Salt: 94.5% |
Table 3 SODIUMNITRATE product performance detect
| Project | Embodiment 1 SODIUMNITRATE product | Technical grade SODIUMNITRATE performance index |
| Sodium-chlor massfraction | 98.6％ | Acceptable industrial salt: 98.5% |
Can be found out by above data, the sodium sulfate product obtained by the inventive method, sodium-chlor product and SODIUMNITRATE product reach the performance requriements of technical grade respectively, can sell as technical grade product.
Claims (9)
1. a recovery and treatment method for high-salt wastewater, is characterized in that: by single vaporization crystallization, cooling crystallization, double evaporation-cooling crystallization, freezing and crystallizing four treatment step reclaim(ed) sulfuric acid sodium, sodium-chlor and SODIUMNITRATE.
2. the recovery and treatment method of a kind of high-salt wastewater according to claim 1, is characterized in that: the concrete steps of described treatment process are,
A, single vaporization crystallization
High-salt wastewater is sent into single vaporization crystallizer to carry out single vaporization and concentrate, thickening temperature is 50 ~ 150 DEG C, be concentrated to crystallization and the solid content of remaining liq is 2 ~ 30% time, at 50 ~ 100 DEG C, carry out solid-liquid separation, obtain sodium sulfate crystal and a mother liquor;
The direct extraction of described sodium sulfate crystal, one time mother liquor enters step B process; At the elutriation leg high-salt wastewater of crystallizer, solid is eluriated, again gained solid is washed at solid-liquid separation process clear water;
B, cooling crystallization
A mother liquor is carried out low temperature crystallization and carries out solid-liquid separation, and recrystallization temperature is-15 ~ 0 DEG C, obtains the mixed salt, the cooling mother liquor that include sal glauberi and two water sodium-chlor;
Described mixed salt is again sent dissolving in high-salt wastewater back to, is carried out circulation and stress process, and cooling mother liquor enters step C process;
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out double evaporation-cooling concentrate, thickening temperature is 50 ~ 150 DEG C, along with the evaporation of moisture, sodium-chlor crystallization in cooling mother liquor and the solid content of remaining liq are when reaching 2 ~ 30%, at 30 ~ 50 DEG C, carry out solid-liquid separation, obtain sodium chloride crystal and secondary mother liquid;
The direct extraction of described sodium chloride crystal, secondary mother liquid enters step D process; At the elutriation leg cooling mother liquor of crystallizer, solid is eluriated, again gained solid is washed at solid-liquid separation process clear water;
D, freezing and crystallizing
Secondary mother liquid is carried out cryogenic freezing crystallization and carries out solid-liquid separation, Tc is-15 ~ 0 DEG C, obtains SODIUMNITRATE crystal and freezing mother liquor;
The direct extraction of described SODIUMNITRATE crystal, freezing mother liquor returns biochemistry pool, and the nitrogenous source as biochemistry pool supplements.
3. the recovery and treatment method of a kind of high-salt wastewater according to claim 2, it is characterized in that: when the organic concentration in described high-salt wastewater, mother liquor, cooling mother liquor, secondary mother liquid and freezing mother liquor is higher than 1000mg/L, directly send biochemical wastewater treatment operation back to, or use gac or catalyzed oxidation to process organism, treat that organic concentration is reduced to below 1000mg/L and enters next treatment step again.
4. the recovery and treatment method of a kind of high-salt wastewater according to claim 2, it is characterized in that: the SODIUMNITRATE crystal of the sodium sulfate crystal of described steps A extraction, the sodium chloride crystal of step C extraction, step D extraction, after washing accordingly and drying treatment, reaches the quality standard of technical grade sodium sulfate, technical grade sodium-chlor, technical grade SODIUMNITRATE respectively.
5. the recovery and treatment method of a kind of high-salt wastewater according to claim 2, it is characterized in that: described single vaporization crystallizer comprises single vaporization device and primary crystallization device, described double evaporation-cooling crystallizer comprises second evaporator and secondary crystal device, and described single vaporization device is the one in the array configuration of a kind of or above-mentioned vaporizer in natural-circulation evaporator, falling-film evaporator, pump feed evaporator, MVR vaporizer, TVR vaporizer.
6. the recovery and treatment method of a kind of high-salt wastewater according to claim 5, it is characterized in that: when in described single vaporization process, double evaporation-cooling process, nodeless mesh is separated out, single vaporization device, second evaporator are falling-film evaporator or natural-circulation evaporator, when having crystallization in single vaporization process, double evaporation-cooling process, single vaporization device, second evaporator are pump feed evaporator.
7. the recovery and treatment method of a kind of high-salt wastewater according to any one of claim 5 or 6, is characterized in that: described single vaporization device and second evaporator are respectively single-effect evaporator, multiple-effect evaporator, MVR vaporizer or TVR vaporizer.
8. the recovery and treatment method of a kind of high-salt wastewater according to claim 2, is characterized in that: the freezing and crystallizing device used in the cooling crystallization device used in described primary crystallization device, step B, secondary crystal device, step D is any one in Oslo crystallizer, draft tube baffle crystallizer, DP crystallizer, Flash Type crystallizer respectively.
9. the recovery and treatment method of a kind of high-salt wastewater according to claim 8, is characterized in that: described step crystallization device is provided with the vertical crystallizer eluriating leg.
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