CN105036222B - A kind of recovery and treatment method of high-salt wastewater - Google Patents
A kind of recovery and treatment method of high-salt wastewater Download PDFInfo
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- CN105036222B CN105036222B CN201510511463.9A CN201510511463A CN105036222B CN 105036222 B CN105036222 B CN 105036222B CN 201510511463 A CN201510511463 A CN 201510511463A CN 105036222 B CN105036222 B CN 105036222B
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Abstract
The invention discloses a kind of recovery and treatment method of high-salt wastewater, it is characterised in that：Crystallized by flush distillation crystallization, cooling crystallization, double evaporation-cooling, four process steps of freezing and crystallizing reclaim sodium sulphate, sodium chloride and sodium nitrate；Can be separately recovered for sodium chloride in high-salt wastewater, sodium sulphate and sodium nitrate by the present invention, sodium chloride, sodium sulphate and the sodium nitrate for obtaining reach technical grade level, can directly recovery or as byproduct sell, the purpose for the treatment of high-salt wastewater is not only reached, meet current Environmental Protection Situation needs, and turn waste into wealth, the recycling of salt is realized, improve the income of factory.
Description
Technical field
The present invention relates to the processing method of waste water, especially a kind of recovery and treatment method of coal chemical industry high-salt wastewater.
Background technology
China is oil-poor, few gas, the energy resource structure of many coals determine that coal is still China's main energy sources at this stage, Coal Chemical Industry
Industry can extract various products from coal, make full use of the value of coal.With continuing to develop for coal chemical industry, also bring
New problem, the generation of coal chemical industry high slat-containing wastewater constrains the continuation development of Coal Chemical Industry, also result in very big environment
Pollution and the wasting of resources.
High-salt wastewater refers to the waste water of the mass content more than or equal to 1.0% of total dissolved solidss and organic matter, including high salt
Sanitary wastewater and high salt industrial wastewater.The main source of high-salt wastewater be directly using seawater industrial production and sanitary sewage,
And food processing factory, pharmaceutical factory, chemical plant, petroleum collection processing industry, the sewage of the natural gas collection generation such as processing industry.
These sewage by the waste water as high-salt wastewater that is obtained after biochemical treatment, except containing organic contamination beyond the region of objective existence in high-salt wastewater,
Also contain substantial amounts of inorganic salts, such as Cl-、SO4 2-、Na+、Ca2+、NO4 -Plasma.High-salt wastewater cannot be completed by biochemical method
Treatment, and materializing strategy process is more complicated, and processing cost is higher, is the generally acknowledged difficult waste water of sewage treatment industry.These
If the unprocessed direct discharge of high-salt wastewater, will certainly be produced to aqueous bio, Drinking Water and industrial and agricultural production with water
High risks.
Treatment technology on high-salt wastewater, has studied decades both at home and abroad, and the method for generally using at present is main
Including biological treatment, ion-exchange, chemical precipitation method and evaporative desalination method etc..Ion-exchange to a certain extent can be with
The purpose of desalination is reached, but the frequent solid suspension because in waste water blocking resin and losing effect, additionally, the method is expensive
And the waste for exchanging is difficult to process.Chemical precipitation method is a kind of traditional method for treating water, and technology is more ripe, investment
Few, treatment is simple, it is only necessary to add medicament, but the more difficult control of the addition of medicament, and medicament excessively, is introduced to waste water
Other impurities, medicament is too low, it is impossible to reach the purpose for the treatment of waste water, additionally, how sediment processes and be also in processed waste water
Restrict one of factor of its development.
In numerous high-salt wastewater treatment technologies, evaporative desalination method has technology maturation, can process that waste water scope is wide, place
The advantages of managing fast speed, energy-conservation, thus there is larger development prospect at home.Evaporative desalination method is to make height with the method for heating
Part water vapor in salt waste water is simultaneously removed, and is that solute is separated out and created conditions to improve the concentration of solution.However, using evaporation
The solid that desalination process is separated out all is the mixed salt comprising various salts simultaneously, and purity is low, it is impossible to industrially reuse, and generally will
Mixed salt is directly discarded or gives the dangerous waste processing mechanism to carry out professional treatment with 300~5000 yuan per ton of price, is so not only carried
Environmental protection pressure high, also considerably increases the cost for wastewater treatment of factory.
The produced sewage in Coal Chemical Industry production process, by biochemical treatment and filters impurity, remaining high-salt wastewater
In mainly include sodium sulphate, sodium chloride, three kinds of salt of sodium nitrate, the mixed salt of these three salt is very difficult to treatment, and these three salt
Usage amount industrially is very big, discards in vain unfortunately.Therefore, sodium sulphate, sodium chloride and the nitre in high-salt wastewater are reclaimed
Sour sodium is significant.
The content of the invention
The technical problem to be solved in the invention is to provide a kind of recovery of the high-salt wastewater produced for coal chemical industry
Processing method, can effectively be recycled by the method to the sodium sulphate in high-salt wastewater, sodium chloride and sodium nitrate,
Substantially reduce environmental protection pressure and cost for wastewater treatment.
In order to solve the above technical problems, the technical solution adopted in the present invention is：
A kind of recovery and treatment method of high-salt wastewater, by flush distillation crystallization, cooling crystallization, double evaporation-cooling crystallize, it is cold
Freeze brilliant four process steps and reclaim sodium sulphate, sodium chloride and sodium nitrate.
Technical solution of the present invention further improvement is that：The processing method is concretely comprised the following steps,
A, flush distillation crystallization
High-salt wastewater feeding flush distillation crystallizer is carried out into flush distillation concentration, thickening temperature is 50~150 DEG C, concentration
To have crystallization separate out and remaining liq solid content be 2~30% when, separation of solid and liquid is carried out at 50~100 DEG C, obtain sulfuric acid
Sodium crystal and a mother liquor；
The sodium sulfate crystal is directly produced, and one time mother liquor enters step B treatment；It is useless with high salt in the elutriation leg of crystallizer
Water is eluriated to solid, and gained solid is washed again with clear water in solid-liquid separation process；
B, cooling crystallization
Mother liquor is carried out into low temperature crystallization and separation of solid and liquid is carried out, recrystallization temperature is -15~0 DEG C, obtains including ten
The mixed salt of aqueous sodium persulfate and two water sodium chloride, cooling mother liquor；
The mixed salt is sent back in high-salt wastewater and dissolves, is circulated recycling again, and cooling mother liquor enters at step C
Reason；
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out into double evaporation-cooling concentration, thickening temperature is 50~150 DEG C, with
The evaporation of moisture, when the solid content of sodium chloride crystallization precipitation and remaining liq in cooling mother liquor reaches 2~30%, 30~50
Separation of solid and liquid is carried out at DEG C, sodium chloride crystal and secondary mother liquid is obtained；
The sodium chloride crystal is directly produced, and secondary mother liquid enters step D treatment；It is female with cooling in the elutriation leg of crystallizer
Liquid is eluriated to solid, and gained solid is washed again with clear water in solid-liquid separation process；
D, freezing and crystallizing
Secondary mother liquid is carried out into cryogenic freezing to crystallize and carry out separation of solid and liquid, crystallization temperature is -15~0 DEG C, obtains nitric acid
Sodium crystal and freezing mother liquor；
The nitric acid sodium crystal is directly produced, and freezing mother liquor returns to biochemistry pool, is supplemented as the nitrogen source of biochemistry pool.
Technical solution of the present invention further improvement is that：The high-salt wastewater, mother liquor, cooling mother liquor, a secondary mother
When organic concentration in liquid and freezing mother liquor is higher than 1000mg/L, biochemical wastewater treatment operation is directly sent back to, or use work
Property charcoal or catalysis oxidation organic matter is processed, treat organic concentration be reduced to below 1000mg/L enter back into it is next treatment step
Suddenly.
Technical solution of the present invention further improvement is that：The sodium sulfate crystal of the step A extraction, step C are produced
Sodium chloride crystal, the nitric acid sodium crystal of step D extraction are by after corresponding washing and dried process, respectively reaching technical grade sulfuric acid
Sodium, industrial grade sodium chloride, the quality standard of industrial grade sodium nitrate.
Technical solution of the present invention further improvement is that：The flush distillation crystallizer is including flush distillation device and once
Crystallizer, the double evaporation-cooling crystallizer includes revaporizer and secondary crystallization device, and the flush distillation device is Natural Circulation
A kind of or above-mentioned evaporator in evaporator, falling film evaporator, forced-circulation evaporator, MVR evaporators, TVR evaporators
One kind in combining form.
Technical solution of the present invention further improvement is that：Nodeless mesh during the flush distillation process, double evaporation-cooling
During precipitation, flush distillation device, revaporizer are falling film evaporator or natural-circulation evaporator, flush distillation process, secondary steaming
When having crystallization to separate out during hair, flush distillation device, revaporizer are forced-circulation evaporator.
Technical solution of the present invention further improvement is that：The flush distillation device and revaporizer are respectively single-action steaming
Hair device, multi-effect evaporator, MVR evaporators or TVR evaporators.
Technical solution of the present invention further improvement is that：The cooling crystallization used in the primary crystallization device, step B
The freezing and crystallizing device used in device, secondary crystallization device, step D is respectively Oslo crystallizers, DTB crystallizers, DP crystallizers, flash distillation
Any one in formula crystallizer.
Technical solution of the present invention further improvement is that：The step crystallization device is provided with eluriating the vertical crystallization of leg
Device.
By adopting the above-described technical solution, the technological progress that the present invention is obtained is：
The invention provides a kind of recovery and treatment method of high-salt wastewater, the high salt for being produced to processes such as Coal Chemical Industries is given up
Water is reclaimed, process conditions simple and stable.By the inventive method, can by the sodium chloride in high-salt wastewater, sodium sulphate and
Sodium nitrate is separately recovered, and sodium chloride, sodium sulphate and the sodium nitrate for obtaining reach technical grade level, can directly recovery or work
Be that byproduct is sold, not only reached the purpose for the treatment of high-salt wastewater, meet current Environmental Protection Situation needs, and change give up into
Treasured, realizes the recycling of salt, improves the income of factory.
The inventive method is circulation process method, and the mixed salt produced in treatment returns to circulation and stress treatment in high-salt wastewater,
Freezing mother liquor returns to double evaporation-cooling Crystallization Procedure, and whole process is in addition to having moisture evaporation, without other sewage discharges, therefore environmental protection
Pressure is die-offed, and without being processed to the payment of dangerous waste processing mechanism again, greatly reduces cost for wastewater treatment.In recycling process
In, for being dissolved in the salt that cannot be separated out completely in mother liquor, finally separated out by constantly enrichment, realize high-salt wastewater
Middle salt is reclaimed to greatest extent.
The present invention is especially set according to the dissolubility property of sodium sulphate, sodium chloride and sodium nitrate.Sodium sulphate it is molten
Dramatically increased with the rising of temperature when Xie Du is below about 40 DEG C, and dropped with the rising of temperature when more than this temperature
It is low, though the solubility of sodium chloride increasing with temperature and being increased slightly, it is influenced by temperature less.Therefore, when reclaiming sodium sulphate,
Using being first concentrated by evaporation and then separating out at relatively high temperatures sodium sulfate crystal by high-salt wastewater, by controlling evaporation endpoint concentration,
Ensure that evaporation endpoint concentration falls in the crystal region of sodium sulphate, there is no sodium chloride to separate out, so as to obtain the sodium sulphate of high-purity.Centrifugation
A mother liquor after separating sodium sulfate separates out the mixed salt of sodium sulphate and sodium chloride by cooling again, further removes remnants'
Sodium sulphate, sodium chloride, nitric acid sodium content are very high in remaining cooling mother liquor after separation of solid and liquid, only contain extremely micro sulfuric acid
Sodium.
, according to sodium chloride and the characteristic of sodium nitrate dissolubility binary phase diagraml, sodium nitrate cementing degree is very high under high temperature for the present invention,
And sodium chloride temperature influence is not obvious, therefore, will cooling mother liquor under high temperature double evaporation-cooling crystallization, be then filtrated to get it is high-purity
The sodium chloride of degree.By controlling evaporation endpoint concentration, it is ensured that evaporation endpoint concentration falls in the crystal region of sodium chloride, does not have sodium nitrate
Separated out with sodium sulphate.Main Salts are sodium nitrate in secondary mother liquid after Isolating chlorinated sodium, now make mother liquor in freezing under low temperature
Crystallization obtains high pure nitric acid sodium, and freezing mother liquor returns to double evaporation-cooling Crystallization Procedure circular treatment.Circulation by said process is past
It is multiple, can be recycled sodium sulphate, sodium chloride and the sodium nitrate of the overwhelming majority in high-salt wastewater.
After high-salt wastewater of the invention is crystallized through flush distillation, in heat filtering under higher temperature, the sulfuric acid of high-purity is obtained
Sodium；Mother liquor cooling crystallization obtains the mixed salt of sodium sulphate and sodium chloride, further removes sodium sulphate, and mixed salt returns to feed reservoir and adjusts
Section Cl-And SO4 2-Ion ratio；Gained cooling mother liquor is crystallized in double evaporation-cooling under high temperature, and subsequent heat filtering obtains high-purity chlorination
Sodium；Secondary mother liquid evaporative crystallization is filtrated to get high-purity sodium nitrate after freezing and crystallizing under low temperature.This technology is using elutriation leg formula
Crystallizing evaporator, can be backwashed with mother liquor or material liquid to it, it is ensured that the crystal grain of extraction is uniform and containing less miscellaneous
Matter.
Organic matter is processed in the present invention, can both ensure the purity and color and luster of salinity, salinity is reached work
Industry level standard, can avoid influenceing evaporation process because organic matter constantly adds up to cause the elevation of boiling point serious again.
When using multi-effect evaporator in step A, optional falling film evaporator, Natural Circulation evaporation when being separated out without crystallization
Any one in device, forced-circulation evaporator, preferably falling film evaporator.Falling film evaporator is with heat exchange area very high and very well
Heat exchange property, and solution internal circulating load very little is especially suitable for the big flush distillation step of evaporation capacity, can effectively accelerate evaporation speed
Degree, reduces evaporation cost.
Double evaporation-cooling crystallizer in step C from any one in forced-circulation evaporator, scrapper thin film evaporator,
It is preferred that forced-circulation evaporator.Forced-circulation evaporator is the evaporator that a kind of heat transfer coefficient is big, resistive connection scar ability is strong, and solution exists
Circulation in equipment relies primarily on the forced flow produced by additionaling power, and circulation rate is general up to 1.5~5 meter per seconds；When following
Be heated when ring liquid flows through heating chamber, then part is evaporated during pressure reduction in separation chamber, will liquid cooling to correspondence
Boiling temperature under pressure, due to circulating pump, the operation of forced-circulation evaporator is substantially unrelated with temperature, and material is again
Circulation rate can be set within the specific limits with accurate adjustment, evaporation rate；Feed liquid is separated again into separator, can be strengthened point
From effect, make integral device that there is larger separation elasticity；Evaporate separate out crystal can by adjust circulation flow rate and
Separated from loop slurry using special separator design, be conducive to processing larger viscosity, easy fouling, the thing of easily crystallization
Material or concentrating degree solution higher, therefore be highly suitable for double evaporation-cooling step and use, sodium chloride crystal can effectively be divided
From.
Used in the cooling crystallization device, secondary crystallization device, the step D that are used in primary crystallization device, step B in the present invention
Freezing and crystallizing device is selected from any in Oslo crystallizers, DTB crystallizers, DP crystallizers, Flash Type crystallizer and its mutation pattern
One kind, is preferably provided with the vertical DTB crystallizers and its mutation for eluriating leg.DTB crystallizers and its mutation pattern are a kind of typical
Magma inner circulation type crystallizer, with good fluid dynamic effect；Pressure head needed for its interior circulation is very low, propeller or
Axial-flow pump works under relatively low rotating speed, so as to greatly reduce the secondary nucleation that collision of the impeller to crystal is brought, and then
Ensure that the crystal produced in crystallizer has larger granularity, and size distribution is good, inwall seldom occur and scab phenomenon；DTB
The crystallizer operation cycle is long, energy consumption is low, reliable, failure is few.The vertical DTB crystallizers for being provided with elutriation leg can be realized continuously
Production operation, realizes the circulation and stress treatment to high-salt wastewater.Vertical elutriation leg can be carried out inverse when crystal is produced with material liquid
To washing, it is ensured that the crystal of extraction contains impurity at least, to reach technical grade.
Brief description of the drawings
The step of Fig. 1 is processing method of the present invention and the schematic diagram of separation product；
Fig. 2 is the concrete technology flow process schematic diagram of embodiment 1；
Wherein, 1, preheater, 2, one effect heating chamber, 3, one effect separation chamber, 4, two effect heating chambers, 5, two effect fractional crystallizations
Device, 6, centrifuge, 7, mother liquor tank, 8, jacket type cooling stirred tank, 9, cooling crystallization centrifuge, 10, cooling mother liquor
Tank, 11, triple effect heating chamber, 12, triple effect fractional crystallization device, 13, indirect condenser, 14, condensate water pot, 15, secondary centrifuging machine,
16th, secondary mother liquid tank, 17, Outer Cooler, 18, Oslo crystallizers, 19, thickener, 20, freezing and crystallizing centrifuge, 21 freezing mother liquors
Tank, 22, high-salt wastewater feed pipe, 23, condensate output transistor road I, 24, steam input pipe road, 25, chilled brine input pipe
Road, 26, sodium sulphate discharge pipe, 27, condensate output transistor road, 28, sodium chloride discharge pipe, 29, recirculated water water supply pipeline,
30th, recirculated water water return pipeline, 31, chilled brine output channel, 32, sodium nitrate discharge pipe.
Black arrow in Fig. 2 represents the trend of high-salt wastewater, and double-head arrow represents cooling water, chilled water, steam, condensed water
Trend.
Specific embodiment
The present invention is described in further details with reference to embodiment and accompanying drawing：
A kind of recovery and treatment method of high-salt wastewater, as shown in figure 1, passing through flush distillation crystallization, cooling crystallization, secondary steaming
Hair crystallization, four process steps of freezing and crystallizing reclaim sodium sulphate, sodium chloride and sodium nitrate.
This recovery and treatment method is concretely comprised the following steps：
A, flush distillation crystallization
The preheated rear feeding flush distillation crystallizer of high-salt wastewater is evaporated concentration, thickening temperature is about 50~150
℃；During this, the water evaporation in high-salt wastewater so that the concentration of wherein salt gradually rises, until separating out now is separated out
Crystal is sal glauberi；When the solid content for being evaporated to remaining liq is 2~30%, the most of sodium sulphate in high-salt wastewater
Gradually crystallization is separated out, and during sodium chloride and sodium nitrate remain in liquid phase.After carrying out separation of solid and liquid under the conditions of 50~100 DEG C, obtain
To the sodium sulfate crystal of high-purity and a mother liquor；
The sodium sulfate crystal separated out in flush distillation crystallization process, first in the elutriation leg high-salt wastewater pair of crystallizer
Solid is eluriated, and gained solid is washed again with clear water in solid-liquid separation process then.The sodium sulphate of gained high-purity
Crystal is directly produced, and after dried process, its purity reaches technical grade, can be used as industrial sulphuric acid sodium again or directly as
Byproduct is sold.
The content of sodium sulphate is relatively low in mother liquor of gained, and feeding step B is further processed, chlorination in adjustment mother liquor
The concentration ratio of sodium and sodium sulphate.
In this step, preferably 50~100 DEG C of flush distillation thickening temperature, most preferably 75 DEG C.It is evaporated to remaining liq
Solid content is preferably 10~30%, most preferably 20%.Preferably 60~80 DEG C, most preferably 70 DEG C of separation of solid and liquid temperature.
B, cooling crystallization
Mother liquor is sent into cooler crystallizer further to be lowered the temperature crystallization, recrystallization temperature is -15 DEG C~0 DEG C；With
Temperature reduction, remaining most of sodium sulphate and partial oxidation sodium can together crystallize precipitation；Being kept for -15 DEG C~0 DEG C carries out solid-liquid
Separating treatment, obtains mixed salt and cooling mother liquor.
The mixed salt is sent back to dissolve and continue cycling through in high-salt wastewater and is recycled again.
Sodium chloride and sodium nitrate concentration are very high in the cooling mother liquor, and the content of sodium sulphate is further reduced to 0.44%~
1.2%, it is ensured that by evaporating into the crystal region of sodium chloride, it is admitted to step C and is further processed.
In this step, preferably -10 DEG C~-2 DEG C, most preferably -5 DEG C of recrystallization temperature.Preferably -10 DEG C of separation of solid and liquid temperature
~-2 DEG C, most preferably -5 DEG C.
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out into double evaporation-cooling concentration, thickening temperature is 50 DEG C~150 DEG C, is protected
The crystal region by evaporating into sodium chloride is demonstrate,proved, with the continuous evaporation of water, the sodium chloride in mother liquor to be cooled gradually crystallizes analysis
Go out, when the solid content for being evaporated to remaining liq is 2~30%, sodium chloride is separated out completely substantially；At a temperature of 30 DEG C~50 DEG C
Processed through separation of solid and liquid, obtain sodium chloride crystal and secondary mother liquid；
The sodium chloride crystal separated out in double evaporation-cooling crystallization process, first in the elutriation leg cooling mother liquor pair of crystallizer
Solid is eluriated, and gained solid is washed again with clear water in solid-liquid separation process then.Gained sodium chloride crystal is direct
Extraction, after dried process, its purity reaches technical grade, can be used as industrial chlorinations sodium again or gone out directly as byproduct
Sell.
Sodium nitrate concentration is very high in the secondary mother liquid, and sodium sulphate and sodium chloride content are extremely low, is admitted to step D and enters to advance
The treatment of one step.
In this step, preferably 80~120 DEG C of double evaporation-cooling thickening temperature, most preferably 100 DEG C.It is evaporated to remaining liq
Solid content is preferably 10~30%, most preferably 20%.Preferably 30~40 DEG C, most preferably 30 DEG C of separation of solid and liquid temperature.
D, freezing and crystallizing
Secondary mother liquid feeding freezing and crystallizing device is carried out into freezing and crystallizing, crystallization temperature is -15 DEG C~0 DEG C；As temperature drops
Low, sodium nitrate crystallization is separated out；Processed by separation of solid and liquid, obtain nitric acid sodium crystal and freezing mother liquor；
Gained nitric acid sodium crystal is directly produced, and after dried process, its purity reaches technical grade, can again as industrial nitre
Sour sodium is sold using or directly as byproduct.In the freezing mother liquor or three common saturated solution, in order to thoroughly reclaim
Product salt therein, therefore freezing mother liquor sent back in double evaporation-cooling operation, continues cycling through and recycled again.
In this step, preferably -15 DEG C~-5 DEG C, most preferably -10 DEG C of crystallization temperature.Preferably -15 DEG C of separation of solid and liquid temperature
~-5 DEG C, most preferably -10 DEG C.
In actual production process, when the low salinity in high-salt wastewater, salt content are below 10%, if being sent directly into
Flush distillation Crystallization Procedure, then the quantity of steam that evaporates consumption is big, steam expense is higher, in order to save evaporation energy consumption, Ke Yixian
Pre-concentration is carried out to high-salt wastewater using MVR evaporators, salt content is reached 20% or so, be re-fed into flush distillation crystallizer,
The energy consumption of circulating treatment procedure can effectively be reduced.
Due to inevitably containing some organic matters in coal chemical industrial waste water, influenced whether if organic matter too high levels
The precipitation of salt.Therefore, needed in actual production process to high-salt wastewater, mother liquor, cooling mother liquor, secondary mother liquid and cold
The content of organics frozen in mother liquor is monitored；When content of organics is higher than 1000mg/L, then need to use activated carbon, activated coke
Or catalysed oxidation processes are processed organic matter, when organic concentration is down to below 1000mg/L, it can be ensured that obtain work
During industry level solid salt, next process step is entered back into, adsorbing the activated carbon or activated coke of organic matter can deliver to boiler burning.Once
Mother liquor, cooling mother liquor, secondary mother liquid and freezing mother liquor are because amount is fewer, it is also contemplated that directly return to biochemical system treatment
COD。
Embodiment 1
The present embodiment be containing sodium sulphate, sodium chloride, the high-salt wastewater of sodium nitrate recovery processing technique, technological process is such as
Shown in Fig. 2.
In the present embodiment, flush distillation crystallization uses economic benefits and social benefits following current flow, and 1st effective evaporator uses falling film evaporator, including
One effect separation chamber 3 and effect heating chamber 2.2nd effect evaporator uses forced-circulation evaporation crystallizer, including two effect fractional crystallization devices 5
With two effect heating chambers 4.
Using jacket type cooling stirred tank 8, refrigerant uses chilled brine to cooling crystallization.
Double evaporation-cooling crystallization uses single-action forced-circulation evaporator, including triple effect fractional crystallization device 12 and triple effect heating chamber
11。
Freezing and crystallizing operation uses external-cooling type Oslo crystallizers, including Outer Cooler 17 and Oslo crystallizers 18.
Flow direction of material：
A, flush distillation crystallization
High-salt wastewater in head tank enters preheater 1 by high-salt wastewater feed pipe 22 first, it is preheated after given
To flush distillation Crystallization Procedure.High-salt wastewater is initially entered in the 1st effective evaporator of falling film evaporator composition, is evaporated concentration,
A part of feed liquid realizes effect interior circulation through an effect circulating pump, and another part feed liquid is crossed and expects what forced-circulation evaporation crystallizer was constituted
Two effect crystallizing evaporators, continue to be concentrated by evaporation.Solid content to remaining liq to be evaporated be 20% when, through a centrifuge 6 from
The heart is separated, and obtains sodium sulfate crystal and a mother liquor.Sodium sulfate crystal is by the directly extraction, scrubbed dry of sodium sulphate discharge pipe 26
Finished product sale is can be used as after dry treatment, a mother liquor enters a mother liquor tank 7 and keeps in.
B, cooling crystallization
A mother liquor in mother liquor tank 7 enters cooling crystallization operation, and mother liquor is delivered to jacket type cooling stirring through pump
Kettle 8, keeping temperature is -15 DEG C~0 DEG C, include the mixed salt of sal glauberi and two water sodium chloride with temperature reduction together
Crystallization is separated out, and mixed salt and cooling mother liquor are obtained through the centrifugation of cooling crystallization centrifuge 9 after.Mixed salt is sent back to head tank dissolving,
It is used to adjust sodium sulphate and sodium chloride ratio in high-salt wastewater, and continues cycling through utilization；Cooling mother liquor enters cooling mother liquor tank 10
It is temporary.
C, double evaporation-cooling crystallization
Cooling mother liquor in cooling mother liquor tank 10 enters double evaporation-cooling Crystallization Procedure, and being delivered to single-action forced circulation through pump steams
Further evaporative crystallization is carried out in the double evaporation-cooling crystallizer that hair device is constituted, it is 20% to be evaporated to the solid content of remaining liq, warp
Triple effect discharging pump is delivered to secondary centrifuging machine 15 and is centrifuged, and separates to obtain sodium chloride crystal and secondary mother liquid.Sodium chloride crystal is passed through
Finished product sale is can be used as after the direct extraction of superchlorination sodium discharge pipe 28, scrubbed dried process；Secondary mother liquid enters secondary
Mother liquor tank 16 is kept in.
D, freezing and crystallizing
Secondary mother liquid in secondary mother liquid tank 16 enters freezing and crystallizing operation, and being delivered to the Oslo with Outer Cooler 17 through pump ties
Brilliant device 18 carries out freezing and crystallizing, and keeping temperature is -15 DEG C~0 DEG C, and nitric acid sodium crystal is gradually separated out with the reduction of temperature, is passed through after
Thickener 19, cold dynamic crystallizer centrifuge 20 centrifugation obtains nitric acid sodium crystal and cold dynamic mother liquor.Nitric acid sodium crystal is by sodium nitrate
Finished product sale is can be used as after the direct extraction of discharge pipe 32, scrubbed dried process；Cold dynamic mother liquor enters cold dynamic mother liquor tank 21.
By continuing cycling through utilization in the cooling mother liquor tank 10 of mother liquor pumped back double evaporation-cooling Crystallization Procedure, thoroughly to reclaim therein
Salt.
Steam flow：
Steam carries out heat exchange condensation by steam input pipe road 24 into the shell side of an effect heating chamber 2, and condensed water is used as warm
Source enters the shell side preheating high-salt wastewater material liquid of preheater 1, and subsequent condensed water delivery pipe road I 23 is delivered to other operations；
The indirect steam produced by an effect separation chamber 3 carries out heat exchange condensation into the shell side of two effect heating chambers 4, and condensed water adds into triple effect
Hot cell 11 makes full use of as thermal source；The indirect steam that two effect fractional crystallization devices 5 are produced is used for double evaporation-cooling Crystallization Procedure (i.e. three
Effect evaporator) thermal source, with triple effect heating chamber 11 exchange heat after condensed water through pipeline send into condensate water pot 14.
Condensation flow to：
Condensed water in condensate water pot 14 is driven by pump, is exported by condensate output transistor road II 27 again, is carried out further
Recycling.After the secondary vapour that triple effect fractional crystallization device 12 is produced is condensed through indirect condenser 13, on-condensible gas is by vacuum pumping
Go out, enter air.
Chilled brine is flowed to：
Chilled brine from chilled brine input channel 25 respectively enters cooling stirred tank 8 and the shell side of Outer Cooler 17 enters
Row cooling down, then directly chilled salt solution output channel 31 is discharged.
Circulating water flow to：
Come self-circulating water water supply pipeline 29 cooling water enter indirect condenser 13 exchange heat after, directly through recirculated water return pipe
Discharge in road 30.
Sodium sulfate crystal, sodium chloride crystal and nitric acid sodium crystal that this technique is produced, after washing and drying, progressive
Can detect, testing result is shown in Table 1, table 2, table 3 respectively.
The sodium sulphate properties of product of table 1 are detected
| Project | The sodium sulphate product of embodiment 1 | Technical grade sulfuric acid sodium performance indications |
| Sodium sulfate quality fraction | 95.8% | III class Grade A：95% |
The sodium chloride properties of product of table 2 are detected
| Project | The sodium chloride product of embodiment 1 | Industrial grade sodium chloride performance indications |
| Sodium chloride mass fraction | 95.2% | Two grades of Exposure to Sunlight Nacls：94.5% |
The sodium nitrate product performance detection of table 3
| Project | The sodium nitrate product of embodiment 1 | Industrial grade sodium nitrate performance indications |
| Sodium chloride mass fraction | 98.6% | Acceptable industrial salt：98.5% |
By data above as can be seen that the sodium sulphate product, sodium chloride product and the nitric acid that are obtained by the inventive method
Sodium product respectively reaches the performance requirement of technical grade, can sell as technical grade product.
Claims (8)
1. a kind of recovery and treatment method of high-salt wastewater, it is characterised in that：By flush distillation crystallization, cooling crystallization, secondary steaming
Hair crystallization, four process steps of freezing and crystallizing reclaim sodium sulphate, sodium chloride and sodium nitrate;
Concretely comprise the following steps,
A, flush distillation crystallization
High-salt wastewater feeding flush distillation crystallizer is carried out into flush distillation concentration, thickening temperature is 50 ~ 150 DEG C, has been concentrated to
Crystallization separate out and remaining liq solid content be 2 ~ 30% when, separation of solid and liquid is carried out at 50 ~ 100 DEG C, obtain sodium sulfate crystal and
Mother liquor；
The sodium sulfate crystal is directly produced, and one time mother liquor enters step B treatment；In the elutriation leg high-salt wastewater pair of crystallizer
Solid is eluriated, and gained solid is washed again with clear water in solid-liquid separation process；
B, cooling crystallization
Mother liquor is carried out into low temperature crystallization and separation of solid and liquid is carried out, recrystallization temperature is -15 ~ 0 DEG C, obtains including ten water sulfuric acid
The mixed salt of sodium and two water sodium chloride, cooling mother liquor；
The mixed salt is sent back in high-salt wastewater and dissolves, is circulated recycling again, and cooling mother liquor enters step C treatment；
C, double evaporation-cooling crystallization
Cooling mother liquor feeding double evaporation-cooling crystallizer is carried out into double evaporation-cooling concentration, thickening temperature is 50 ~ 150 DEG C, with moisture
Evaporation, when the sodium chloride crystallization in cooling mother liquor is separated out and the solid content of remaining liq reaches 2 ~ 30%, enter at 30 ~ 50 DEG C
Row separation of solid and liquid, obtains sodium chloride crystal and secondary mother liquid；
The sodium chloride crystal is directly produced, and secondary mother liquid enters step D treatment；In the elutriation leg cooling mother liquor pair of crystallizer
Solid is eluriated, and gained solid is washed again with clear water in solid-liquid separation process；
D, freezing and crystallizing
Secondary mother liquid is carried out into cryogenic freezing to crystallize and carry out separation of solid and liquid, crystallization temperature is -15 ~ -5 DEG C, obtain sodium nitrate brilliant
Body and freezing mother liquor；
The nitric acid sodium crystal is directly produced, and freezing mother liquor returns to biochemistry pool, is supplemented as the nitrogen source of biochemistry pool.
2. the recovery and treatment method of a kind of high-salt wastewater according to claim 1, it is characterised in that：The high-salt wastewater,
When organic concentration in mother liquor, cooling mother liquor, secondary mother liquid and a freezing mother liquor is higher than 1000mg/L, sewage is directly sent back to
Biochemical treatment operation, or organic matter is processed using activated carbon or catalysis oxidation, treat that organic concentration is reduced to
Below 1000mg/L enters back into next process step.
3. the recovery and treatment method of a kind of high-salt wastewater according to claim 1, it is characterised in that：The step A extraction
Sodium sulfate crystal, the sodium chloride crystal of step C extraction, step D extraction nitric acid sodium crystal is by corresponding washing and dries
After treatment, technical grade sulfuric acid sodium, industrial grade sodium chloride, the quality standard of industrial grade sodium nitrate are respectively reached.
4. the recovery and treatment method of a kind of high-salt wastewater according to claim 1, it is characterised in that：The flush distillation knot
Brilliant device includes flush distillation device and primary crystallization device, and the double evaporation-cooling crystallizer includes revaporizer and secondary crystallization device,
The flush distillation device is natural-circulation evaporator, falling film evaporator, forced-circulation evaporator, MVR evaporators, TVR evaporators
In a kind of or above-mentioned evaporator combining form in one kind.
5. the recovery and treatment method of a kind of high-salt wastewater according to claim 4, it is characterised in that：The flush distillation
When nodeless mesh is separated out during journey, double evaporation-cooling, flush distillation device, revaporizer are that falling film evaporator or Natural Circulation are evaporated
Device, when having crystallization to separate out during flush distillation process, double evaporation-cooling, flush distillation device, revaporizer steam for forced circulation
Hair device.
6. the recovery and treatment method of a kind of high-salt wastewater according to any one of claim 4 or 5, it is characterised in that：It is described
Flush distillation device and revaporizer are respectively single effect evaporator, multi-effect evaporator, MVR evaporators or TVR evaporators.
7. the recovery and treatment method of a kind of high-salt wastewater according to claim 1, it is characterised in that：The primary crystallization
The freezing and crystallizing device used in the cooling crystallization device, secondary crystallization device, the step D that are used in device, step B is respectively Oslo crystallizations
Any one in device, DTB crystallizers, DP crystallizers, Flash Type crystallizer.
8. the recovery and treatment method of a kind of high-salt wastewater according to claim 7, it is characterised in that：The step crystallization device
It is provided with eluriating the vertical crystallizer of leg.
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